CN110550866B - Method for preparing high-strength glazed microcrystalline glass from granite waste - Google Patents
Method for preparing high-strength glazed microcrystalline glass from granite waste Download PDFInfo
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- CN110550866B CN110550866B CN201910878793.XA CN201910878793A CN110550866B CN 110550866 B CN110550866 B CN 110550866B CN 201910878793 A CN201910878793 A CN 201910878793A CN 110550866 B CN110550866 B CN 110550866B
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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
- 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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- 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
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/91—Use of waste materials as fillers for mortars or concrete
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Abstract
The invention provides a method for preparing high-strength glazed microcrystalline glass from granite waste. The method comprises the steps of firstly, screening and grading granite waste, and ball-milling in water to form slurry; removing iron-containing mineral components in the slurry through magnetic separation, and drying to obtain granite powder; then, uniformly mixing the granite powder and other additives by ball milling to obtain mixed powder, and pressing the mixed powder into a biscuit in a mould; and finally, preparing the high-strength glazed microcrystalline glass by adopting a two-step method: firstly, high-temperature glaze firing; secondly, the sintered body is crystallized at low temperature. The high-strength glazed microcrystalline glass has the characteristics of low production energy consumption, good glaze glossiness and high bending strength, and is expected to be applied to high-grade building decoration materials.
Description
Technical Field
The invention relates to microcrystalline glass, in particular to a method for preparing microcrystalline glass.
Background
Granite is one of the most widely distributed rocks on earth, belonging to the invaded rock in the rock pulp. Its main components are feldspar and quartz, and its secondary components mainly include magnetite and mica. It is hard, difficult to weather, the color is various, have strong chemical resistance, therefore become a high-quality building material. With the development of modern economy and construction, the demand for granite is increasing, thereby promoting the mass mining and processing of granite. However, the average utilization rate of granite is only about 30%. In the process, a large amount of block and powder waste materials are generated, which have great influence on the natural ecological environment and the residential environment of residents and also cause serious waste of non-renewable natural resources.
Granite waste is mainly applied to the fields of permeable bricks, Concrete, cement, geopolymer and ceramic additives (Arel H S, et al. semi-green environmental Materials from wall cement by conditioning the environmental, environmental and health concerns: A review [ J ] Structural concern, 2019,20(1): 455. 470.), but the waste addition amount is less (less than or equal to 20%), the additional value is low (Ghorbani S, et al. mechanical and environmental concerns of Concrete with wall cement product as a partial overlay environmental concern, 2019,194: the industrial waste is applied to poor industrial utilization.
The microcrystalline glass is a polycrystalline solid material containing a large number of microcrystalline phases and glass phases, which is prepared by controlling crystallization behaviors in a heat treatment process of base glass with a certain composition. The microcrystalline glass is different from ceramic and glass. Although the structure and the performance of the material are different from those of ceramics and glass, the material has the basic performance of the glass and the polycrystalline characteristic of the ceramics, and becomes a unique novel material. Although the microcrystalline glass is researched and applied in many fields, the defect of high energy consumption still exists in the actual production, and the energy conservation and emission reduction are not facilitated.
Researchers have now attempted to produce microcrystalline glass from granite waste by a fusion process. Kang et Al prepared microcrystalline glass by melting granite waste material in an amount of 50-68 wt% (Crystallization modifier and properties of CaO-MgO-Al)2O3-SiO2 glass-ceramics synthesized from granite wastes[J]Journal of Non-Crystalline Solids,2017,457: 111-.
Disclosure of Invention
Aiming at the problems in the background art, the invention provides a method for preparing high-strength glazed microcrystalline glass from granite waste.
The invention provides a method for preparing high-strength glazed microcrystalline glass from granite waste, which comprises the following steps:
(1) crushing granite waste, and mixing with water to form slurry;
(2) removing iron-containing mineral components in the slurry, and then drying to obtain granite powder;
(3) adding an aluminum source, waste glass powder, dolomite and boric acid into granite powder, and uniformly mixing to obtain mixed powder; wherein the mixed powder comprises the following components in percentage by mass: 80-90% of granite powder, 0.5-5% of aluminum source, 1-5% of waste glass powder, 5-10% of dolomite and 0.5-5% of boric acid;
(4) and placing the mixed powder in a die, pressing the mixed powder into a biscuit, and sintering the biscuit by a two-step method to obtain the high-strength glazed microcrystalline glass.
Further, the mixed powder comprises the following components in percentage by mass: 85% of granite powder, 3% of aluminum source, 3% of waste glass powder, 6% of dolomite and 3% of boric acid.
Furthermore, the aluminum source is at least one of boehmite, gibbsite and bayer stone, and the waste glass powder is soda-lime-silicate glass powder with the particle size of 200 meshes.
Further, the two-step process comprises: the first step is high-temperature glaze firing, wherein the sintering temperature range is 1100-1300 ℃, and 1200 ℃ is preferred; the second step is low-temperature heat treatment crystallization, wherein the heat treatment temperature range is 800-1000 ℃, and the preferred temperature is 800 ℃.
Further, the mixing in the step (1) and the step (3) is ball milling mixing.
The beneficial effects of the invention include:
(1) a large amount of waste raw materials are used, including granite waste and waste glass powder, the raw materials are very wide in source, and the production cost is greatly reduced;
(2) preparing the glaze microcrystalline glass by adopting a two-step method, wherein the first step is high-temperature glaze firing to form a high-glossiness glaze; the second step is low temperature crystallization to obtain high crystallinity and high strength microcrystalline glass;
(3) the surface of the prepared high-strength glazed microcrystalline glass has beautiful luster, and the grinding and polishing are not needed in the later period, so that the production period can be shortened, and the production cost can be reduced; the volume density of the high-strength glazed microcrystalline glass is 219-245kg/m3The bending strength is 100-135 MPa, the water absorption is 0.05-0.45%, the Vickers hardness is 3.9-5.5 GPa, and the surface glossiness of the glaze surface is 65-78 GU, so that the ceramic glaze is expected to be applied to high-grade building decoration materials;
(4) the method has the characteristics of low energy consumption, energy conservation and environmental protection, and is suitable for large-scale and high-added-value utilization of granite waste.
Drawings
Fig. 1 is an XRD spectrum of the high-strength glazed glass ceramic prepared in example 1.
Fig. 2 is an FESEM topography of the high strength glazed glass ceramic prepared in example 1.
Fig. 3 is a digital photograph of a high strength glazed glass ceramic prepared in example 1.
Detailed Description
In order to make the technical solution and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments, which are only for illustrating the present invention and are not to be construed as limiting the present invention.
Example 1
The raw materials are selected according to the mass percentage: 85% of granite waste, 3% of boehmite, 3% of waste glass powder, 6% of dolomite and 3% of boric acid. The preparation method comprises the following steps of:
(1) sieving and grading the granite waste, adding water and ball milling to form slurry;
(2) carrying out magnetic separation on the slurry, removing iron-containing mineral components in the slurry, and drying to obtain granite powder;
(3) adding boehmite, waste glass powder, dolomite and boric acid into granite powder, ball-milling and uniformly mixing, and sieving by a standard sieve mesh with 325 meshes to obtain mixed powder;
(4) putting the mixed powder into a die, pressing the mixed powder into a biscuit, heating the biscuit from room temperature to 1200 ℃, keeping the temperature for 2 hours at the heating rate of 30 ℃/min, and cooling the biscuit in the furnace to room temperature to obtain a sintered body; and (3) heating the obtained sintered body from room temperature to 800 ℃, heating at the rate of 10 ℃/min, keeping the temperature for 2h, and cooling in a furnace to room temperature to obtain the high-strength glazed glass ceramics.
Analyzing the crystal phase structure of the glazed microcrystalline glass by utilizing X-ray diffraction (XRD), measuring the volume density and the water absorption rate of the glazed microcrystalline glass by utilizing an Archimedes drainage method, observing the appearance of the glazed microcrystalline glass by utilizing a Field Emission Scanning Electron Microscope (FESEM), measuring the bending strength of the glazed microcrystalline glass by utilizing a three-point bending strength test method, and measuring the hardness of the glazed microcrystalline glass by utilizing a Vickers hardness tester; the glaze gloss was measured using a surface gloss meter.
The volume density of the high-strength glazed microcrystalline glass prepared by the embodiment is 225kg/m3The bending strength is 110MPa, the water absorption is 0.20 percent, the Vickers hardness is 4.5GPa, and the glaze glossiness is 73 GU. From fig. 1, it can be seen that the crystal phase of the glazed glass-ceramic is anorthite and quartz. As can be seen from FIG. 2, the glazed microcrystalline glass is composed of a glass phase and a microcrystalline phase, and the microcrystalline phase is mainly in the form of strips, rods and equiaxed shapes. It can be seen from fig. 3 that the prepared microcrystalline glass has good glaze luster.
Example 2
The raw materials are selected according to the mass percentage: 90% of granite waste, 5% of waste glass powder and 5% of dolomite. The preparation method comprises the following steps of:
(1) sieving and grading the granite waste, adding water and ball milling to form slurry;
(2) carrying out magnetic separation on the slurry, removing iron-containing mineral components in the slurry, and drying to obtain granite powder;
(3) adding waste glass powder and dolomite into granite powder, ball-milling and uniformly mixing, and sieving by using a standard sieve mesh with the size of 325 meshes to obtain mixed powder;
(4) putting the mixed powder into a die, pressing the mixed powder into a biscuit, heating the biscuit from room temperature to 1200 ℃, keeping the temperature for 2 hours at the heating rate of 30 ℃/min, and cooling the biscuit in the furnace to room temperature to obtain a sintered body; and (3) heating the obtained sintered body from room temperature to 800 ℃, heating at the rate of 10 ℃/min, keeping the temperature for 2h, and cooling in a furnace to room temperature to obtain the high-strength glazed glass ceramics.
Analyzing the crystal phase structure of the glazed microcrystalline glass by utilizing X-ray diffraction (XRD), measuring the volume density and the water absorption rate of the glazed microcrystalline glass by utilizing an Archimedes drainage method, observing the appearance of the glazed microcrystalline glass by utilizing a Field Emission Scanning Electron Microscope (FESEM), measuring the bending strength of the glazed microcrystalline glass by utilizing a three-point bending strength test method, and measuring the hardness of the glazed microcrystalline glass by utilizing a Vickers hardness tester; the glaze gloss was measured using a surface gloss meter.
The high-strength glazed microcrystalline glass prepared by the embodiment has the volume density of 220kg/m3100MPa of bending strength and water absorptionThe rate is 0.30 percent, the Vickers hardness is 5.0GPa, and the glaze surface glossiness is 65 GU.
Example 3
The raw materials are selected according to the mass percentage: 80% of granite waste, 5% of boehmite, 5% of waste glass powder, 5% of dolomite and 5% of boric acid. The preparation method comprises the following steps of:
(1) sieving and grading the granite waste, adding water and ball milling to form slurry;
(2) carrying out magnetic separation on the slurry, removing iron-containing mineral components in the slurry, and drying to obtain granite powder;
(3) adding boehmite, waste glass powder, dolomite and boric acid into granite powder, ball-milling and uniformly mixing, and sieving by a standard sieve mesh with 325 meshes to obtain mixed powder;
(4) putting the mixed powder into a die, pressing the mixed powder into a biscuit, heating the biscuit from room temperature to 1150 ℃, keeping the temperature for 2h at the heating rate of 30 ℃/min, and cooling the biscuit in the furnace to room temperature to obtain a sintered body; and (3) heating the obtained sintered body from room temperature to 900 ℃, heating at the rate of 10 ℃/min, keeping the temperature for 2h, and cooling in a furnace to room temperature to obtain the high-strength glazed glass ceramics.
Analyzing the crystal phase structure of the glazed microcrystalline glass by utilizing X-ray diffraction (XRD), measuring the volume density and the water absorption rate of the glazed microcrystalline glass by utilizing an Archimedes drainage method, observing the appearance of the glazed microcrystalline glass by utilizing a Field Emission Scanning Electron Microscope (FESEM), measuring the bending strength of the glazed microcrystalline glass by utilizing a three-point bending strength test method, and measuring the hardness of the glazed microcrystalline glass by utilizing a Vickers hardness tester; the glaze gloss was measured using a surface gloss meter.
The high-strength glazed microcrystalline glass prepared by the embodiment has the volume density of 230kg/m3The bending strength is 105MPa, the water absorption is 0.25 percent, the Vickers hardness is 4.0GPa, and the glaze surface glossiness is 70 GU.
In conclusion, the usage amount of the granite waste in the method is 80-90%, so that the utilization rate of the waste is obviously improved; the waste glass powder is used as a sintering aid, so that the compactness of a sintered body is improved, and the content of a glass phase is improved, and the waste glass powder is used for basic glass; dolomite is an additive that controls the crystallinity of the glass-ceramic. Through a two-step method, a large amount of glass phases are generated through the first step of high-temperature glaze firing, and a glaze surface with good glossiness is formed; and the second step of low temperature crystallization heat treatment, which aims at crystallization and converting the glass phase into a crystal phase. The crystal phase composition of the finally prepared glaze microcrystalline glass is any two or more than two of anorthite, diopside and quartz. The invention utilizes granite waste to the maximum extent to prepare the high-strength glazed microcrystalline glass, solves the problems of environmental protection and resource utilization of the granite waste, and can be widely applied to the field of building materials.
Claims (7)
1. A method for preparing high-strength glazed microcrystalline glass from granite waste comprises the following steps:
(1) crushing granite waste, and mixing with water to form slurry;
(2) removing iron-containing mineral components in the slurry, and then drying to obtain granite powder;
(3) adding an aluminum source, waste glass powder, dolomite and boric acid into granite powder, and uniformly mixing to obtain mixed powder; wherein the mixed powder comprises the following components in percentage by mass: 80-90% of granite powder, 0.5-5% of aluminum source, 1-5% of waste glass powder, 5-10% of dolomite and 0.5-5% of boric acid;
(4) and placing the mixed powder in a die, pressing the mixed powder into a biscuit, and sintering the biscuit by a two-step method to obtain the high-strength glazed microcrystalline glass.
2. The method of claim 1, wherein: the mixed powder comprises the following components in percentage by mass: 85% of granite powder, 3% of aluminum source, 3% of waste glass powder, 6% of dolomite and 3% of boric acid.
3. The method of claim 1, wherein: the aluminum source is at least one of boehmite, gibbsite and bayer stone, and the waste glass powder is soda-lime-silicate glass powder with the particle size of 200 meshes.
4. The method of claim 1, wherein: the two-step method comprises the following steps: the first step is high-temperature glaze firing, wherein the sintering temperature range is 1100-1300 ℃; the second step is low-temperature heat treatment crystallization, wherein the heat treatment temperature range is 800-1000 ℃.
5. The method of claim 4, wherein: the two-step method comprises the following steps: the first step is high-temperature glaze firing, wherein the sintering temperature is 1200 ℃; the second step is low temperature heat treatment crystallization, the heat treatment temperature is 800 ℃.
6. The method of claim 1, wherein: the mixing in the step (1) and the step (3) is ball milling mixing.
7. The high-strength glazed microcrystalline glass obtained by the method of any one of claims 1 to 6.
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| CN101851063A (en) * | 2010-05-21 | 2010-10-06 | 郑州大学 | Technology for preparing microcrystal glass by utilizing blast furnace water granulated slag and coal ash |
| CN106430984A (en) * | 2016-09-22 | 2017-02-22 | 陕西科技大学 | Method for preparing microcrystal wollastonite glass from wollastonite |
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