CN110436789B - Microcrystalline foam glass and preparation method thereof - Google Patents
Microcrystalline foam glass and preparation method thereof Download PDFInfo
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- CN110436789B CN110436789B CN201910725625.7A CN201910725625A CN110436789B CN 110436789 B CN110436789 B CN 110436789B CN 201910725625 A CN201910725625 A CN 201910725625A CN 110436789 B CN110436789 B CN 110436789B
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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
- C03B19/00—Other methods of shaping glass
- C03B19/08—Other methods of shaping glass by foaming
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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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- 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
- C03C11/00—Multi-cellular glass ; Porous or hollow glass or glass particles
- C03C11/007—Foam glass, e.g. obtained by incorporating a blowing agent and heating
Abstract
The invention provides microcrystalline foam glass and a preparation method thereof, wherein the preparation method comprises the following steps: s1, preparing basic glass powder: ball-milling and uniformly mixing the raw materials, placing the mixture in a frit furnace, and performing melting, clarification, homogenization, water quenching and grinding to obtain basic glass powder; the raw materials comprise the following components in percentage by mass: 70-80% of gold tailings, 5-15% of blast furnace slag, 2-9% of bentonite, 5-10% of soda ash, 0.2-0.5% of antimony trioxide and 1-3% of titanium dioxide; s2, preparing microcrystalline foam glass: ball-milling and uniformly mixing the basic glass powder prepared in the step S1 with silicon carbide micro powder and sodium fluosilicate, and then feeding the mixture into a high-temperature furnace for firing; the mass percentages of the components in the mixture are as follows: 94.8 to 98.5 percent of basic glass powder, 0.2 to 0.6 percent of silicon carbide micro powder and 1 to 5 percent of sodium fluosilicate. The method provided by the invention takes gold tailings as a main raw material to prepare the microcrystalline foam glass with excellent performance, and provides a new idea for large-scale and high-value utilization of the tailings.
Description
Technical Field
The invention relates to the field of green building materials, in particular to microcrystalline foam glass and a preparation method thereof.
Background
The gold tailings mostly belong to silicate tailings and mainly comprise SiO2And Al2O3Gold tailings mostly exist in a powder form, the stockpiling of the gold tailings occupies a large amount of land, land resources are wasted, serious accidents such as collapse, landslide and dam collapse are easy to happen to the stockpiled tailings, and serious casualties and economic loss are causedLoss, and along with the increase of tailing storehouse dam body, the potential safety hazard increases day by day, remains a large amount of medicaments in the gold tailings simultaneously, such as poisonous and harmful substance such as cyanide, chloride, infiltration groundwater pollutes the water source to the tailings of piling do produces a large amount of dusts, causes the wider pollution under wind-force promotes, how to realize the waste utilization of gold tailings becomes a problem that awaits a moment urgently to solve.
Meanwhile, China is currently in a key stage of economic transformation and upgrading, the urbanization rate is increased by more than one fourth in nearly thirty years, the area of buildings is greatly increased and reaches the top of the world, the total amount of building energy consumption in China exceeds 27%, and newly built houses in urban and rural areas are nearly 20 hundred million square meters every year, more than 80% of the buildings are high-energy-consumption buildings, wherein air-conditioning and heating energy consumption is the main reason of building energy consumption and accounts for about 60% -70%, and in order to reasonably utilize resources and reduce energy consumption, building energy conservation becomes the key for reducing energy consumption, the core of building energy conservation in China is to reform building enclosure structures and heating systems, particularly the improvement of energy conservation technology of building outer wall enclosure structures, and the updating of heat insulation materials has great significance to the reduction of society and building energy consumption.
In view of the renewal of building materials and the realization of the recycling of wastes, the invention provides a method for preparing microcrystalline foam by taking gold tailings as a main raw material.
Disclosure of Invention
The invention aims to provide a method for preparing microcrystalline foam glass by using gold tailings, and the microcrystalline foam glass prepared by the method has the characteristics of light weight, high strength, heat preservation, heat insulation and high added value of products.
The invention provides microcrystalline foam glass which is prepared from the following raw materials in percentage by mass: 94.8 to 98.5 percent of basic glass powder, 0.2 to 0.6 percent of silicon carbide micro powder and 1 to 5 percent of sodium fluosilicate;
the base glass powder is prepared from the following raw materials in percentage by mass: 70-80% of gold tailings, 5-15% of blast furnace slag, 2-9% of bentonite, 5-10% of soda ash, 0.2-0.5% of antimony trioxide and 1-3% of titanium dioxide.
The invention also provides a method for preparing microcrystalline foam by adopting the raw materials, which comprises the following steps:
s1, preparing basic glass powder: ball-milling and uniformly mixing gold tailings, blast furnace slag, bentonite, soda ash, antimony trioxide and titanium dioxide serving as production raw materials, putting the mixture into a frit furnace, and performing melting, clarification, homogenization, water quenching and grinding to obtain base glass powder;
s2, preparing microcrystalline foam glass: ball-milling and uniformly mixing the basic glass powder prepared in the step S1 with silicon carbide micro powder and sodium fluosilicate, and then feeding the mixture into a high-temperature furnace for firing;
preferably, in the step S1, the temperature is 1450-.
Preferably, before the mixture is fired in step S2, the method further includes the following steps: and putting the mixture after ball milling into a corundum-mullite sagger with the inner wall and the bottom surface paved with alumina silicate paper with the thickness of 1mm and the refractoriness of 1260 ℃, and paving and compacting the mixture to obtain the mixture with the volume of 40-50% of the volume of the sagger.
Preferably, the step S2 further includes: sending the mixture into a high temperature furnace, heating up to 400-minus-one-year-old-year 600 ℃ from room temperature at the heating rate of 10-15 ℃/min, heating up to 700-minus-one-year-old-year 800 ℃ at the heating rate of 5-10 ℃/min, then heating up to 950-minus-one-year-old-year 980 ℃ at the heating rate of 10-20 ℃/min, then rapidly cooling down to 600-650 ℃ at the speed of 15-20 ℃/min, preserving heat for 1-2h, heating up to 750-800 ℃ at the heating rate of 5-10 ℃/min, preserving heat for 2-3 h.
Compared with the prior art, the invention has the following technical effects:
(1) the invention utilizes other batch materials such as gold tailings to prepare the base glass, through crushing and grinding, make glass powder, mix with foaming agent, fluxing agent, prepare and get the foamed glass of microcrystal through the secondary heating, the said method raw materials of the invention are easy to get, the utilization rate of solid waste is high, the product has light, high-strength characteristic, can apply to the field such as freezer, building wall, underground oil pipeline;
(2) the method takes the gold tailings as the main raw material to prepare the microcrystalline foam glass with excellent performance, wherein the addition amount of the gold tailings is close to 80 percent, a large amount of tailings are consumed, the damage of the tailings to the ecological environment is reduced, and a new idea is provided for the large-scale and high-value utilization of the tailings;
(3) the volume density of the microcrystalline foam glass prepared by the invention is 400-750kg/m3The compression strength is 5-15Mpa, the average bubble diameter is 0.1-0.5mm, the mechanical property index of the product is excellent, and the pore distribution is uniform.
Drawings
FIG. 1 is an XRD pattern of a microcrystalline foam glass made from gold tailings in accordance with example 1 of the present invention;
fig. 2 is a microstructure diagram of the pores of the microcrystalline foam glass made from the gold tailings of the present invention in example 1.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The invention provides microcrystalline foam glass taking gold tailings as a main raw material and a preparation method thereof, wherein the gold tailings comprise SiO (silicon dioxide) in percentage by mass2：65％-75％；Al2O3：10％-20％；CaO：0.5％-3％；MgO：0.1％-2％；Fe2O3：2％-5％；K2O：2％-5％；Na2O：0.1％-2％；TiO2: 0.1% -2%; 1% -5% of others; the gold tailings used in examples 1-3 were derived from gold tailings from the golden three-mountain island, Shandong.
Example 1
A preparation method of microcrystalline foam glass comprises the following steps:
mixing raw materials: weighing raw materials according to mass percentage, and putting the raw materials into a ball mill to be uniformly mixed, wherein the raw materials comprise the following components: 70% of gold tailings, 15% of blast furnace slag, 8.8% of bentonite, 5% of soda ash, 0.2% of antimony trioxide and 1% of titanium dioxide;
preparing base glass powder: placing the uniformly mixed raw materials into a frit furnace, setting the temperature to 1450 ℃, keeping the temperature for 1.5h, clarifying and homogenizing the molten raw materials, then performing water quenching, and placing the obtained basic glass into a ball mill for ball milling for 1h to obtain basic glass powder;
3) mixing glass powder: putting the base glass powder prepared in the step 2), the silicon carbide micro powder and the sodium fluosilicate into a ball mill for ball milling for 1h, and uniformly mixing, wherein the mixture comprises the following components in percentage by mass: 95% of base glass powder, 0.2% of silicon carbide micro powder and 4.8% of sodium fluosilicate; placing the mixture after ball milling into a corundum-mullite sagger with the inner wall and the bottom surface paved with aluminum silicate paper with the thickness of 1mm and the refractoriness of 1260 ℃, and paving and compacting, wherein the volume of the mixture is 40% of the volume of the sagger;
4) preparing microcrystalline foam glass: and (3) feeding the mixture green body in the step 3) into a high-temperature furnace, heating to 400 ℃ from room temperature at a heating rate of 10 ℃/min, heating to 700 ℃ at a heating rate of 5 ℃/min, heating to 950 ℃ at a heating rate of 10 ℃/min, rapidly cooling to 600 ℃ at a heating rate of 15 ℃/min, preserving heat for 1h, heating to 750 ℃ at a heating rate of 5 ℃/min, preserving heat for 2h, and cooling to room temperature along with the furnace.
The XRD pattern of the microcrystalline foam glass prepared in the example is shown in figure 1, the microstructure of the air holes is shown in figure 2, and the volume density of the foam glass is 750kg/m after being tested3The compressive strength is 15 MPa.
Example 2
A method for preparing a microcrystalline bubble comprises the following steps:
1) mixing raw materials: weighing 75% of gold tailings, 10% of blast furnace slag, 5.7% of bentonite, 7% of soda ash, 0.3% of antimony trioxide and 2% of titanium dioxide according to mass percentage, and putting the mixture into a ball mill to be uniformly mixed;
2) preparing base glass powder; placing the uniformly mixed raw materials into a frit furnace, setting the temperature at 1470 ℃, keeping the temperature for 1.7h, clarifying and homogenizing the molten raw materials, then performing water quenching, and placing the obtained basic glass into a ball mill for ball milling for 1h to obtain basic glass powder;
3) mixing glass powder: putting the base glass powder prepared in the step 2), the silicon carbide micro powder and the sodium fluosilicate into a ball mill for ball milling for 1h, and uniformly mixing, wherein the mixture comprises the following components in percentage by mass: 96.6% of base glass powder, 0.4% of silicon carbide micro powder and 3% of sodium fluosilicate; putting the mixture after ball milling into a corundum-mullite sagger with 1mm thick aluminum silicate paper with the refractoriness of 1260 ℃, and spreading and compacting the mixture in the sagger, wherein the compacted volume is 45 percent of the volume of the sagger;
4) preparing microcrystalline foam glass: and (3) feeding the mixture green body in the step 3) into a high-temperature furnace, heating up to 500 ℃ from room temperature at a heating rate of 13 ℃/min, heating up to 750 ℃ at a heating rate of 7 ℃/min, heating up to 970 ℃ at a heating rate of 15 ℃/min, rapidly cooling to 630 ℃ at a heating rate of 17 ℃/min, preserving heat for 1.5h, heating up to 770 ℃ at a heating rate of 7 ℃/min, preserving heat for 2.5h, and cooling to room temperature along with the furnace.
The volume density of the microcrystalline foam glass prepared by the embodiment is 640kg/m3The compressive strength is 13 MPa.
Example 3
A preparation method of microcrystalline foam glass comprises the following steps:
1) mixing raw materials: weighing 80% of gold tailings, 5% of blast furnace slag, 2% of bentonite, 9.5% of soda ash, 0.5% of antimony trioxide and 3% of titanium dioxide according to mass percentage, and putting the mixture into a ball mill to be uniformly mixed;
2) preparing base glass powder: placing the uniformly mixed raw materials into a frit furnace, setting the temperature to be 1500 ℃, keeping the temperature for 2 hours, clarifying and homogenizing the molten raw materials, then performing water quenching, and placing the obtained basic glass into a ball mill for ball milling for 1 hour to obtain basic glass powder;
3) mixing glass powder: putting the base glass powder prepared in the step 2), the silicon carbide micro powder and the sodium fluosilicate into a ball mill for ball milling for 1h, and uniformly mixing, wherein the mixture comprises the following components in percentage by mass: 98.4% of basic glass powder, 0.6% of silicon carbide micro powder and 1% of sodium fluosilicate; placing the mixture after ball milling into a corundum-mullite sagger with 1mm thick aluminum silicate paper with the refractoriness of 1260 ℃ paved on the inner wall and the bottom surface, and paving and compacting the mixture, wherein the compacted volume is 50% of the volume of the sagger;
4) preparing microcrystalline foam glass: and (3) feeding the mixture green body in the step 3) into a high-temperature furnace, heating to 600 ℃ from room temperature at a heating rate of 15 ℃/min, heating to 800 ℃ at a heating rate of 10 ℃/min, heating to 980 ℃ at a heating rate of 20 ℃/min, rapidly cooling to 650 ℃ at a heating rate of 20 ℃/min, preserving heat for 2h, heating to 800 ℃ at a heating rate of 10 ℃/min, preserving heat for 3h, and cooling to room temperature along with the furnace.
The volume density of the microcrystalline foam glass prepared by the embodiment is 400kg/m3The compressive strength is 5 MPa.
The technical idea of the present invention is described in the above technical solutions, and the protection scope of the present invention is not limited thereto, and any changes and modifications made to the above technical solutions according to the technical essence of the present invention belong to the protection scope of the technical solutions of the present invention.
Claims (4)
1. The microcrystalline foam glass is characterized by being prepared from the following raw materials in percentage by mass: 94.8 to 98.5 percent of basic glass powder, 0.2 to 0.6 percent of silicon carbide micro powder and 1 to 5 percent of sodium fluosilicate;
the base glass powder is prepared from the following raw materials in percentage by mass: 70-80% of gold tailings, 5-15% of blast furnace slag, 2-9% of bentonite, 5-10% of soda ash, 0.2-0.5% of antimony trioxide and 1-3% of titanium dioxide.
2. A method for preparing the microcrystalline foam glass of claim 1, comprising the steps of:
s1, preparing basic glass powder: ball-milling and uniformly mixing production raw materials including gold tailings, blast furnace slag, bentonite, soda ash, antimony trioxide and titanium dioxide, placing the mixture into a frit furnace, setting the temperature to 1450 and 1500 ℃, keeping the temperature for 1-2 hours, and melting, clarifying, homogenizing, water quenching and grinding the raw materials to obtain base glass powder;
s2, preparing microcrystalline foam glass: and (2) ball-milling and uniformly mixing the basic glass powder prepared in the step S1, silicon carbide micro powder and sodium fluosilicate, then sending the mixture into a high-temperature furnace for firing, heating the mixture from room temperature to 400-600 ℃ at the heating rate of 10-15 ℃/min, heating the mixture to 700-800 ℃ at the heating rate of 5-10 ℃/min, then heating the mixture to 950-980 ℃, rapidly cooling the mixture to 600-650 ℃ at the heating rate of 10-20 ℃/min, preserving heat for 1-2h, heating the mixture to 750-800 ℃ at the heating rate of 5-10 ℃/min, preserving heat for 2-3h, and then cooling the mixture to room temperature along with the furnace.
3. The method according to claim 2, wherein before the step S2 of firing the mixed material, the method further comprises the steps of: and putting the mixture after ball milling into a corundum-mullite sagger with the inner wall and the bottom surface paved with aluminum silicate paper with the thickness of 1mm and the refractoriness of 1260 ℃, paving and compacting, wherein the volume of the compacted mixture is 40-50% of the volume of the sagger.
4. The preparation method as claimed in claim 2, wherein the volume density of the prepared microcrystalline foam glass is 400-750kg/m3And the compressive strength is 5-15 Mpa.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910725625.7A CN110436789B (en) | 2019-08-07 | 2019-08-07 | Microcrystalline foam glass and preparation method thereof |
| PCT/CN2019/101867 WO2021022588A1 (en) | 2019-08-07 | 2019-08-22 | Microcrystalline foam glass and preparation method therefor |
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| CN201910725625.7A CN110436789B (en) | 2019-08-07 | 2019-08-07 | Microcrystalline foam glass and preparation method thereof |
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| CN110436789A CN110436789A (en) | 2019-11-12 |
| CN110436789B true CN110436789B (en) | 2020-11-24 |
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| CN112340999A (en) * | 2020-11-18 | 2021-02-09 | 肖德才 | Insulation board and preparation method thereof |
| CN113754285B (en) * | 2021-08-23 | 2023-08-25 | 湖州大享玻璃制品有限公司 | Bentonite tailing-based ecological glass ceramic |
| CN114620938B (en) * | 2022-03-17 | 2024-03-01 | 河南省高新技术实业有限公司 | Hierarchical porous glass ceramic and preparation method thereof |
| CN114573227B (en) * | 2022-03-22 | 2024-02-20 | 洛阳理工学院 | Calendaring photovoltaic glass clarifying agent and application thereof |
| CN115490429B (en) * | 2022-08-19 | 2023-11-03 | 湖南兆湘光电高端装备研究院有限公司 | Composition for preparing microcrystalline glass, microcrystalline glass and preparation method and application thereof |
| CN115636588A (en) * | 2022-10-26 | 2023-01-24 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for preparing microcrystalline glass by extracting titanium tailings |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE19702560A1 (en) * | 1997-01-24 | 1998-07-30 | Erhard Lehmann | Evaluating used cathode ray tube glass e.g. from television(s) |
| CN101717195A (en) * | 2009-11-10 | 2010-06-02 | 陕西科技大学 | Method for producing microcrystalling foam glass with gold tail ore |
| CN101913771A (en) * | 2010-07-05 | 2010-12-15 | 清华大学 | Method for preparing microcrystalline porous foam glass tube |
| CN105819695A (en) * | 2016-05-05 | 2016-08-03 | 内蒙古科技大学 | Cyanide tailing foam microcrystalline glass and preparation method thereof |
-
2019
- 2019-08-07 CN CN201910725625.7A patent/CN110436789B/en active Active
- 2019-08-22 WO PCT/CN2019/101867 patent/WO2021022588A1/en active Application Filing
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE19702560A1 (en) * | 1997-01-24 | 1998-07-30 | Erhard Lehmann | Evaluating used cathode ray tube glass e.g. from television(s) |
| CN101717195A (en) * | 2009-11-10 | 2010-06-02 | 陕西科技大学 | Method for producing microcrystalling foam glass with gold tail ore |
| CN101913771A (en) * | 2010-07-05 | 2010-12-15 | 清华大学 | Method for preparing microcrystalline porous foam glass tube |
| CN105819695A (en) * | 2016-05-05 | 2016-08-03 | 内蒙古科技大学 | Cyanide tailing foam microcrystalline glass and preparation method thereof |
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| WO2021022588A1 (en) | 2021-02-11 |
| CN110436789A (en) | 2019-11-12 |
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