CN112499975A - Method for preparing mullite porous glass ceramic by using molybdenum tailings - Google Patents
Method for preparing mullite porous glass ceramic by using molybdenum tailings Download PDFInfo
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- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 title claims abstract description 48
- 229910052750 molybdenum Inorganic materials 0.000 title claims abstract description 48
- 239000011733 molybdenum Substances 0.000 title claims abstract description 48
- 239000000919 ceramic Substances 0.000 title claims abstract description 41
- 239000005373 porous glass Substances 0.000 title claims abstract description 41
- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 title claims abstract description 32
- 229910052863 mullite Inorganic materials 0.000 title claims abstract description 32
- 238000000034 method Methods 0.000 title claims abstract description 29
- 239000006121 base glass Substances 0.000 claims abstract description 15
- 239000002994 raw material Substances 0.000 claims abstract description 14
- 239000011521 glass Substances 0.000 claims description 33
- 239000000203 mixture Substances 0.000 claims description 33
- 238000002156 mixing Methods 0.000 claims description 24
- 239000003795 chemical substances by application Substances 0.000 claims description 22
- 239000010881 fly ash Substances 0.000 claims description 18
- 235000019738 Limestone Nutrition 0.000 claims description 17
- 239000006028 limestone Substances 0.000 claims description 17
- 239000002245 particle Substances 0.000 claims description 17
- 239000000292 calcium oxide Substances 0.000 claims description 13
- 238000002360 preparation method Methods 0.000 claims description 13
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical group [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 12
- 235000015895 biscuits Nutrition 0.000 claims description 12
- 238000004321 preservation Methods 0.000 claims description 12
- 238000003825 pressing Methods 0.000 claims description 12
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 11
- 238000010438 heat treatment Methods 0.000 claims description 11
- 239000002667 nucleating agent Substances 0.000 claims description 11
- 239000002131 composite material Substances 0.000 claims description 10
- 238000000227 grinding Methods 0.000 claims description 10
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 9
- 229920002134 Carboxymethyl cellulose Polymers 0.000 claims description 9
- 239000001768 carboxy methyl cellulose Substances 0.000 claims description 9
- 235000010948 carboxy methyl cellulose Nutrition 0.000 claims description 9
- 239000008112 carboxymethyl-cellulose Substances 0.000 claims description 9
- 238000010304 firing Methods 0.000 claims description 9
- 239000010439 graphite Substances 0.000 claims description 9
- 229910002804 graphite Inorganic materials 0.000 claims description 9
- 239000000843 powder Substances 0.000 claims description 9
- 229910021538 borax Inorganic materials 0.000 claims description 8
- 239000004328 sodium tetraborate Substances 0.000 claims description 8
- 235000010339 sodium tetraborate Nutrition 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 6
- 229910052593 corundum Inorganic materials 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
- 238000010791 quenching Methods 0.000 claims description 6
- 230000000171 quenching effect Effects 0.000 claims description 6
- 238000005303 weighing Methods 0.000 claims description 6
- 229910001845 yogo sapphire Inorganic materials 0.000 claims description 6
- KKCBUQHMOMHUOY-UHFFFAOYSA-N Na2O Inorganic materials [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 claims description 3
- 239000003153 chemical reaction reagent Substances 0.000 claims 1
- 239000002699 waste material Substances 0.000 abstract description 6
- 230000008901 benefit Effects 0.000 abstract description 4
- 239000002253 acid Substances 0.000 abstract description 2
- 239000003513 alkali Substances 0.000 abstract description 2
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 6
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 5
- 238000005245 sintering Methods 0.000 description 5
- UQGFMSUEHSUPRD-UHFFFAOYSA-N disodium;3,7-dioxido-2,4,6,8,9-pentaoxa-1,3,5,7-tetraborabicyclo[3.3.1]nonane Chemical compound [Na+].[Na+].O1B([O-])OB2OB([O-])OB1O2 UQGFMSUEHSUPRD-UHFFFAOYSA-N 0.000 description 4
- 239000013078 crystal Substances 0.000 description 3
- CHWRSCGUEQEHOH-UHFFFAOYSA-N potassium oxide Chemical compound [O-2].[K+].[K+] CHWRSCGUEQEHOH-UHFFFAOYSA-N 0.000 description 3
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 239000002241 glass-ceramic Substances 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000002910 solid waste Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229910021532 Calcite Inorganic materials 0.000 description 1
- 239000004566 building material Substances 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000010459 dolomite Substances 0.000 description 1
- 229910000514 dolomite Inorganic materials 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000011494 foam glass Substances 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 238000005065 mining Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 229910001950 potassium oxide Inorganic materials 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
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Classifications
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B11/00—Pressing molten glass or performed glass reheated to equivalent low viscosity without blowing
-
- 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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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Chemical & Material Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Dispersion Chemistry (AREA)
- Crystallography & Structural Chemistry (AREA)
- Ceramic Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Compositions Of Oxide Ceramics (AREA)
Abstract
The invention provides a method for preparing mullite porous glass ceramic by using molybdenum tailings; the method comprises the following steps: (1) pretreating raw materials; (2) preparing base glass; (3) and (3) preparing the mullite porous glass ceramic. The performance parameters of the mullite porous glass ceramic sample prepared by the invention are as follows: the compressive strength is 32.4MPa, the porosity is 21.3 percent, and the density is 2.2g/cm31.15GPa of Vickers hardness, 0.17 percent of acid-resistant mass loss rate and 0.19 percent of alkali-resistant mass loss rate. The backup method only uses the molybdenum tailings as the main raw material, realizes effective utilization of waste secondary resources, changes waste into valuable, turns harm into benefit, simultaneously enlarges the raw material source for preparing the porous glass ceramic, and is beneficial to wider application of the porous glass ceramic.
Description
Technical Field
The invention belongs to the technical field of solid waste mineral deep processing and environmental protection; in particular to a method for preparing mullite porous glass ceramic by using molybdenum tailings.
Background
Molybdenum ore resources in China are rich, ore components are complex, tailings produced after mining are large in stockpiling, land resources are invaded, the ecological environment is polluted, molybdenum tailings mainly comprise calcite, dolomite and the like except a very small amount of molybdenum-containing ore, and the main components of the molybdenum tailings are SiO2(the mass fraction is close to 80%), and the content of other impurities is low, and the impurities mainly comprise metal oxides such as iron oxide, aluminum oxide, potassium oxide and the like. Therefore, a tailings resource utilization way is sought, the additional value of the tailings is improved, and the method becomes a research hotspot for treating the tailings pollution at present.
The porous glass ceramic is a novel functional material developed on the basis of foam glass, and consists of three parts, namely a glass phase, crystals and air holes, wherein the crystals are distributed in a glass matrix containing a plurality of air holes to form a glass-crystal interwoven structure, so that the porous glass ceramic has the advantages of lighter weight and higher compressive resistance than microcrystalline glass, and has excellent performances of low density, high strength, low thermal conductivity, strong chemical stability and the like, thereby being widely applied to the fields of chemical industry, heat preservation and insulation, building materials and the like. The tailings are resources which are misplaced, and the molybdenum tailings are used for preparing the mullite porous glass ceramic, so that waste is changed into valuable, and the method is an embodiment for building an environment-friendly society.
Disclosure of Invention
The invention aims to provide a method for preparing mullite porous glass ceramic by using molybdenum tailings.
The invention is realized by the following technical scheme:
the invention relates to a method for preparing mullite porous glass ceramic by using molybdenum tailings, which comprises the following steps:
(1) pretreatment of raw materials
Molybdenum tailings, limestone (CaO analytically pure) and fly ash (Al)2O3Analytically pure) is ground to below 200 meshes;
(2) preparation of base glass
Weighing the following components in parts by weight:
40-60 parts of molybdenum tailings, namely,
fly ash or Al2O315 to 25 portions of analytically pure,
25-35 parts of limestone or CaO analytically pure,
pouring the components into a mixing tank for mixing, then putting the mixture into a crucible, heating the mixture in a muffle furnace, preserving heat, then taking the crucible for water quenching to obtain glass particles, drying the glass particles, and then grinding the glass particles to obtain base glass; the obtained basic glass component is 42-47% SiO2、2.3％-2.7％Fe2O3、25％-30％％Al2O3、1.2％-1.6％K2O、0.2％-0.7％Na2O、0.05％-0.15％MgO、20％-25％CaO、0.2％-0.7％TiO2
(3) Preparation of mullite porous glass ceramic
Adding a composite pore-forming agent (graphite accounts for 5-15% of the mass of the basic glass powder, carboxymethyl cellulose accounts for 5-15% of the mass of the basic glass powder, and the like), a fluxing agent (anhydrous sodium carbonate or borax accounts for 1-2% of the mass of the basic glass powder or a mixture of the anhydrous sodium carbonate and the borax accounts for 1-2% of the mass of the basic glass powder), and a nucleating agent (Fe)2O3Or TiO21-2 percent of the base glass powder or Fe2O3With TiO2The mixture accounts for 1 to 2 percent of the mass of the basic glass powder, the mixture is put into a die and is dried and pressed under the pressing pressure of 5 to 20MPa to obtain a biscuit, and then the biscuit is put into a box body and is kept warm at the sintering temperature in a muffle furnace to sinter the porous glass ceramic sample.
Preferably, in the step (1), SiO in the molybdenum tailings2The mass percentage of the components is 70-85 percent; the mass percent of CaO in the limestone is 50-60%; al in the fly ash2O3The mass percentage is 30-40%.
Preferably, in the step (2), the time for pouring into the mixing tank for mixing is 20min-40 min.
Preferably, in the step (2), the temperature for heating in the muffle furnace is 1300-1400 ℃.
Preferably, in the step (2), the temperature is maintained in the muffle furnace for 60-120 min.
Preferably, in the step (3), the composite pore-forming agent is a mixture of graphite and carboxymethyl cellulose, the fluxing agent is anhydrous sodium carbonate or borax or a mixture of the anhydrous sodium carbonate and the borax, and the nucleating agent is Fe2O3Or TiO2Or a mixture of both.
Preferably, in step (3), the specification of the mold is: 10mm by 50 mm.
Preferably, in the step (3), the firing temperature is 800 ℃ to 1040 ℃.
Preferably, in the step (3), the heat preservation time is 60min-150 min.
The invention has the following advantages:
the mullite porous glass ceramic sample prepared by the method provided by the invention is tested as follows: the compressive strength is 32.4MPa, the porosity is 21.3 percent, and the density is 2.2g/cm31.15GPa of Vickers hardness, 0.17 percent of acid-resistant mass loss rate and 0.19 percent of alkali-resistant mass loss rate.
The backup method only uses the molybdenum tailings as the main raw material, realizes effective utilization of waste secondary resources, changes waste into valuable, turns harm into benefit, simultaneously enlarges the raw material source for preparing the porous glass ceramic, and is beneficial to wider application of the porous glass ceramic.
Drawings
FIG. 1 is a process flow diagram of a method according to the present invention.
Detailed Description
The present invention will be described in detail with reference to specific examples. It should be noted that the following examples are only illustrative of the present invention, but the scope of the present invention is not limited to the following examples.
Example 1
The embodiment of the invention provides a method for preparing mullite porous glass ceramic by using molybdenum tailings, which comprises the following steps:
(1) pretreatment of raw materials
Molybdenum tailings, limestone (CaO analytically pure) and fly ash (Al)2O3Analytically pure) are respectively ground to below 200 meshes;
(2) preparation of base glass
Weighing the following components in parts by weight:
50 parts of the molybdenum tailings,
20 parts of fly ash, namely 20 parts of fly ash,
30 parts of limestone, namely 30 parts of limestone,
the processed raw materials are weighed according to the formula of the basic glass, and the proportion is 45 percent of SiO2、2.5％Fe2O3、27％Al2O3、1.4％K2O、0.5％Na2O、0.1％MgO、23％CaO、0.5％TiO2Mixing the raw materials in a mixing tank for 30min, then putting the raw materials into a crucible, putting the crucible into a muffle furnace, heating to 1400 ℃, preserving heat for 90min, then taking the crucible for water quenching to obtain glass particles, drying and then grinding to obtain the base glass.
(3) Preparation of mullite porous glass ceramic
And (3) uniformly mixing the basic glass powder prepared in the step (2), a pore-forming agent, a fluxing agent and a nucleating agent, putting the mixture into a mould with the thickness of 10mm multiplied by 50mm, carrying out dry pressing under a certain pressing pressure to obtain a biscuit, putting the biscuit into a box body, and carrying out heat preservation for 120min in a muffle furnace at the firing temperature of 1000 ℃ to fire the porous glass ceramic sample.
Example 2
The embodiment relates to a method for preparing mullite glass ceramics by using molybdenum tailings, which comprises the following steps:
(1) pretreatment of raw materials
Grinding molybdenum tailings, limestone and fly ash to below 200 meshes;
(2) preparation of base glass
Weighing the following components in parts by weight:
40 parts of the molybdenum tailings, namely 40 parts of molybdenum tailings,
fly ash or Al2O3The sample was analyzed for 25 parts by weight,
35 portions of limestone or CaO analytically pure,
pouring the components into a mixing tank for mixing, then putting the mixture into a crucible, heating the mixture in a muffle furnace, preserving heat, then taking the crucible for water quenching to obtain glass particles, drying the glass particles, and then grinding the glass particles to obtain base glass;
in the step (1), SiO in the molybdenum tailings2The mass percentage of the components is 70-85 percent; the mass percent of CaO in the limestone is 50-60%; al in the fly ash2O3The mass percentage is 30-40%.
In the step (2), the mixture is poured into a mixing tank for mixing for 20min to 40min, the mixture is placed in a muffle furnace for heating at 1300 ℃ to 1400 ℃, and the mullite porous glass ceramic is placed in the step (3) for preparation
Adding composite pore-forming agent (graphite 5-15%, carboxymethyl cellulose 5-15%), fluxing agent (anhydrous sodium carbonate or borax or mixture of the two 1-2%), nucleating agent (Fe)2O3Or TiO2Or 1% -2%) of the above-mentioned two materials, placing them into a mould, dry-pressing and forming under the pressing pressure of 5MPa-20MPa to obtain biscuit, then placing the biscuit into a box body, at the firing temperature in muffle furnace, making heat preservation and firingPorous glass ceramic samples were made.
The heat preservation time in a muffle furnace is 60min-120 min.
In the step (3), the composite pore-forming agent is a mixture of graphite and carboxymethyl cellulose, the fluxing agent is anhydrous sodium carbonate, and the nucleating agent is Fe2O3The specification of the die is as follows: 10mm multiplied by 50mm, the firing temperature is 800-1040 ℃, and the heat preservation time is 60-150 min.
Example 3
The embodiment relates to a method for preparing mullite porous glass ceramic by using molybdenum tailings, which comprises the following steps:
(1) pretreatment of raw materials
Grinding molybdenum tailings, limestone and fly ash to below 200 meshes;
(2) preparation of base glass
Weighing the following components in parts by weight:
60 parts of the molybdenum tailings, namely 60 parts of molybdenum tailings,
fly ash or Al2O315 parts of the mixture is analyzed and purified,
25 portions of limestone or CaO analytically pure,
pouring the components into a mixing tank for mixing, then putting the mixture into a crucible, heating the mixture in a muffle furnace, preserving heat, then taking the crucible for water quenching to obtain glass particles, drying the glass particles, and then grinding the glass particles to obtain base glass;
(3) preparation of mullite porous glass ceramic
Adding composite pore-forming agent (graphite 5-15%, carboxymethyl cellulose 5-15%), fluxing agent (anhydrous sodium carbonate 1-2%), nucleating agent (Fe)2O31% -2%), placing the mixture into a die, performing dry pressing under the pressing pressure of 5-20 MPa to obtain a biscuit, then placing the biscuit into a box body, preserving heat at the sintering temperature in a muffle furnace, and sintering the porous glass ceramic sample.
In the step (1), SiO in the molybdenum tailings2The mass percentage of the components is 70-85 percent; in the limestoneThe mass percent of CaO is 50 percent to 60 percent; al in the fly ash2O3The mass percentage is 30-40%.
In the step (2), the mixture is poured into a mixing tank for mixing for 20min-40min, the heating temperature in a muffle furnace is 1300-1400 ℃, and the heat preservation time in the muffle furnace is 60min-120 min.
In the step (3), the composite pore-forming agent is a mixture of graphite and carboxymethyl cellulose, the fluxing agent is anhydrous sodium carbonate, and the nucleating agent is Fe2O3The specification of the die is as follows: 10mm multiplied by 50mm, the firing temperature is 800-1040 ℃, and the heat preservation time is 60-150 min.
Example 4
The embodiment relates to a method for preparing mullite porous glass ceramic by using molybdenum tailings, which comprises the following steps:
(1) pretreatment of raw materials
Grinding molybdenum tailings, limestone and fly ash to below 200 meshes;
(2) preparation of base glass
Weighing the following components in parts by weight:
45 parts of molybdenum tailings, namely 45 parts of molybdenum tailings,
fly ash or Al2O3The sample was analyzed for 25 parts by weight,
30 portions of limestone or CaO analytically pure,
pouring the components into a mixing tank for mixing, then putting the mixture into a crucible, heating the mixture in a muffle furnace, preserving heat, then taking the crucible for water quenching to obtain glass particles, drying the glass particles, and then grinding the glass particles to obtain base glass;
(3) preparation of mullite porous glass ceramic
Adding composite pore-forming agent (graphite 5-15%, carboxymethyl cellulose 5-15%), fluxing agent (anhydrous sodium carbonate or borax or mixture of the two 1-2%), nucleating agent (Fe)2O3Or TiO2Or the mixture of the two is 1 percent to 2 percent), putting the mixture into a mould, and pressing the mixture at the pressure of 5MPa to 20MPaAnd (3) dry pressing under a pressing force to obtain a biscuit, then putting the biscuit into a box body, keeping the temperature at the sintering temperature in a muffle furnace, and sintering the porous glass ceramic sample.
In the step (1), SiO in the molybdenum tailings2The mass percentage of the components is 70-85 percent; the mass percent of CaO in the limestone is 50-60%; al in the fly ash2O3The mass percentage is 30-40%.
In the step (2), the mixture is poured into a mixing tank for mixing for 20min-40min, the heating temperature in a muffle furnace is 1300-1400 ℃, and the heat preservation time in the muffle furnace is 60min-120 min.
In the step (3), the composite pore-forming agent is a mixture of graphite and carboxymethyl cellulose, the fluxing agent is anhydrous sodium carbonate, the nucleating agent is Fe2O3, and the specification of the mold is as follows: 10mm multiplied by 50mm, the firing temperature is 800-1040 ℃, and the heat preservation time is 60-150 min.
The preparation methods of the above examples 1 to 4 are shown in FIG. 1, and the products obtained in examples 1 to 4 of the present invention were subjected to the performance test, and the results are shown in Table 1.
TABLE 1
The method for preparing the mullite porous glass ceramic by using the molybdenum tailings which are solid wastes realizes changing waste into valuable, has simple process, low cost and low energy consumption, and provides an effective way for the comprehensive utilization of the molybdenum tailings.
The foregoing description of specific embodiments of the present invention has been presented. It is to be understood that the present invention is not limited to the specific embodiments described above, and that various changes or modifications may be made by one skilled in the art within the scope of the appended claims without departing from the spirit of the invention.
Claims (9)
1. A method for preparing mullite porous glass ceramic by using molybdenum tailings is characterized by comprising the following steps:
(1) pretreatment of raw materials
Analyzing and purifying molybdenum tailings, limestone or CaO, fly ash or Al2O3Carrying out powder grinding treatment on the analytical reagent until the particle size is below 200 meshes;
(2) preparation of base glass
Weighing the following components in parts by weight:
40-60 parts of molybdenum tailings, namely,
fly ash or Al2O315 to 25 portions of analytically pure,
25-35 parts of limestone or CaO analytically pure,
pouring the components into a mixing tank for mixing, then putting the mixture into a crucible, heating the mixture in a muffle furnace, preserving heat, then taking the crucible for water quenching to obtain glass particles, drying the glass particles, and then grinding the glass particles to obtain base glass; the obtained basic glass comprises the following components: 42% -47% SiO2、2.3％-2.7％Fe2O3、25％-30％％Al2O3、1.2％-1.6％K2O、0.2％-0.7％Na2O、0.05％-0.15％MgO、20％-25％CaO、0.2％-0.7％TiO2；
(3) Preparation of mullite porous glass ceramic
Adding a composite pore-forming agent, a fluxing agent and a nucleating agent into the basic glass powder, adding a small amount of water, uniformly mixing, putting into a mold, carrying out dry pressing forming under the pressing pressure of 5MPa-20MPa to obtain a biscuit, then putting the biscuit into a box body, carrying out heat preservation at the firing temperature in a muffle furnace, and firing the mullite porous glass ceramic sample.
2. The method for preparing mullite porous glass ceramic by using molybdenum tailings as claimed in claim 1, wherein in the step (1), SiO in the molybdenum tailings2The mass percentage of the components is 70-85 percent; the mass percent of CaO in the limestone is 50-60%; al in the fly ash2O3The mass percentage is 30-40%.
3. The method for preparing mullite porous glass ceramic by using molybdenum tailings as claimed in claim 1, wherein in the step (2), the time for pouring into the mixing tank for mixing is 20min-40 min.
4. The method for preparing mullite porous glass ceramic by using molybdenum tailings as claimed in claim 1, wherein in the step (2), the temperature for heating in a muffle furnace is 1300-1400 ℃.
5. The method for preparing the mullite porous glass ceramic by using the molybdenum tailings as claimed in claim 1, wherein in the step (2), the temperature of the mullite porous glass ceramic is kept in a muffle furnace for 60-120 min.
6. The method for preparing mullite porous glass ceramic by using molybdenum tailings as claimed in claim 1, wherein in the step (3), the composite pore-forming agent is graphite accounting for 5% -15% of the basic glass percentage and carboxymethyl cellulose accounting for 5% -15%; the fluxing agent is anhydrous sodium carbonate accounting for 1-2 percent of the basic glass percentage, borax accounting for 1-2 percent of the basic glass percentage, or a mixture of the anhydrous sodium carbonate and the borax accounting for 1-2 percent of the basic glass percentage; the nucleating agent is Fe accounting for 1% -2% of the base glass2O3Or 1% -2% TiO2Or 1% -2% of the mixture of the two.
7. The method for preparing mullite porous glass ceramic by using molybdenum tailings as claimed in claim 1, wherein in the step (3), the specification of the mold is as follows: 10mm by 50 mm.
8. The method for preparing mullite porous glass ceramic by using molybdenum tailings as claimed in claim 1, wherein in the step (3), the firing temperature is 800-1040 ℃.
9. The method for preparing mullite porous glass ceramic by using molybdenum tailings as claimed in claim 1, wherein in the step (3), the heat preservation time is 60min to 150 min.
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