CN108483921B - Iron tailing composite microcrystalline glass and preparation method thereof - Google Patents
Iron tailing composite microcrystalline glass and preparation method thereof Download PDFInfo
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- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 title claims abstract description 128
- 239000011521 glass Substances 0.000 title claims abstract description 96
- 229910052742 iron Inorganic materials 0.000 title claims abstract description 64
- 239000002131 composite material Substances 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 239000010410 layer Substances 0.000 claims abstract description 61
- 239000002344 surface layer Substances 0.000 claims abstract description 56
- 239000000758 substrate Substances 0.000 claims abstract description 21
- 238000002844 melting Methods 0.000 claims abstract description 18
- 230000008018 melting Effects 0.000 claims abstract description 18
- 239000000843 powder Substances 0.000 claims description 47
- 238000000227 grinding Methods 0.000 claims description 32
- 239000002994 raw material Substances 0.000 claims description 19
- 239000002241 glass-ceramic Substances 0.000 claims description 18
- 238000010438 heat treatment Methods 0.000 claims description 16
- 239000013078 crystal Substances 0.000 claims description 14
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 14
- 239000008187 granular material Substances 0.000 claims description 13
- 238000000034 method Methods 0.000 claims description 11
- 238000007873 sieving Methods 0.000 claims description 10
- 238000001035 drying Methods 0.000 claims description 9
- 229910021532 Calcite Inorganic materials 0.000 claims description 8
- 239000007788 liquid Substances 0.000 claims description 8
- 239000010453 quartz Substances 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- ADCOVFLJGNWWNZ-UHFFFAOYSA-N antimony trioxide Inorganic materials O=[Sb]O[Sb]=O ADCOVFLJGNWWNZ-UHFFFAOYSA-N 0.000 claims description 7
- 239000000126 substance Substances 0.000 claims description 7
- DLHONNLASJQAHX-UHFFFAOYSA-N aluminum;potassium;oxygen(2-);silicon(4+) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[Al+3].[Si+4].[Si+4].[Si+4].[K+] DLHONNLASJQAHX-UHFFFAOYSA-N 0.000 claims description 5
- NWXHSRDXUJENGJ-UHFFFAOYSA-N calcium;magnesium;dioxido(oxo)silane Chemical compound [Mg+2].[Ca+2].[O-][Si]([O-])=O.[O-][Si]([O-])=O NWXHSRDXUJENGJ-UHFFFAOYSA-N 0.000 claims description 5
- 229910052637 diopside Inorganic materials 0.000 claims description 5
- 238000005485 electric heating Methods 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- 238000005303 weighing Methods 0.000 claims description 5
- 229910052656 albite Inorganic materials 0.000 claims description 4
- 238000011049 filling Methods 0.000 claims description 4
- 238000010791 quenching Methods 0.000 claims description 4
- 230000000171 quenching effect Effects 0.000 claims description 4
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 3
- 238000007605 air drying Methods 0.000 claims description 3
- 238000007664 blowing Methods 0.000 claims description 3
- 239000010433 feldspar Substances 0.000 claims description 3
- 229940072033 potash Drugs 0.000 claims description 3
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Substances [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims description 3
- 235000015320 potassium carbonate Nutrition 0.000 claims description 3
- 238000012216 screening Methods 0.000 claims description 3
- SZVJSHCCFOBDDC-UHFFFAOYSA-N iron(II,III) oxide Inorganic materials O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 claims description 2
- KKCBUQHMOMHUOY-UHFFFAOYSA-N Na2O Inorganic materials [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 claims 4
- 239000000463 material Substances 0.000 abstract description 7
- 238000005034 decoration Methods 0.000 abstract description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 230000007547 defect Effects 0.000 abstract description 2
- 239000002585 base Substances 0.000 description 16
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 14
- 238000002425 crystallisation Methods 0.000 description 13
- 230000008025 crystallization Effects 0.000 description 13
- 239000011787 zinc oxide Substances 0.000 description 7
- 239000000395 magnesium oxide Substances 0.000 description 6
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 6
- 230000008569 process Effects 0.000 description 5
- 238000005520 cutting process Methods 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 239000000377 silicon dioxide Substances 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 229910000831 Steel Inorganic materials 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 229910052681 coesite Inorganic materials 0.000 description 3
- 229910052906 cristobalite Inorganic materials 0.000 description 3
- 239000010959 steel Substances 0.000 description 3
- 229910052682 stishovite Inorganic materials 0.000 description 3
- 229910052905 tridymite Inorganic materials 0.000 description 3
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 229910052783 alkali metal Inorganic materials 0.000 description 2
- 150000001340 alkali metals Chemical class 0.000 description 2
- 238000005452 bending Methods 0.000 description 2
- 238000004040 coloring Methods 0.000 description 2
- 230000003247 decreasing effect Effects 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000009776 industrial production Methods 0.000 description 2
- GALOTNBSUVEISR-UHFFFAOYSA-N molybdenum;silicon Chemical compound [Mo]#[Si] GALOTNBSUVEISR-UHFFFAOYSA-N 0.000 description 2
- 238000010899 nucleation Methods 0.000 description 2
- 230000006911 nucleation Effects 0.000 description 2
- 238000005498 polishing Methods 0.000 description 2
- 230000004913 activation Effects 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 238000004031 devitrification Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 230000009477 glass transition Effects 0.000 description 1
- 238000010348 incorporation Methods 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000011089 mechanical engineering Methods 0.000 description 1
- 238000010309 melting process Methods 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 238000004886 process control Methods 0.000 description 1
- 238000012797 qualification Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- YEAUATLBSVJFOY-UHFFFAOYSA-N tetraantimony hexaoxide Chemical compound O1[Sb](O2)O[Sb]3O[Sb]1O[Sb]2O3 YEAUATLBSVJFOY-UHFFFAOYSA-N 0.000 description 1
- 239000012856 weighed raw material Substances 0.000 description 1
- 230000002087 whitening effect Effects 0.000 description 1
- 229910052882 wollastonite Inorganic materials 0.000 description 1
- 239000010456 wollastonite Substances 0.000 description 1
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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
-
- 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
-
- 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
-
- 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
-
- 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
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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)
- Glass Compositions (AREA)
Abstract
The invention discloses iron tailing composite microcrystalline glass which comprises a substrate layer and a surface layer which are combined together, wherein the substrate layer contains iron tailings, and the surface layer does not contain the iron tailings. The surface layer and the base layer have different crystalline phases. The glass melting point of the surface layer is lower than that of the substrate layer. The invention also discloses a preparation method of the iron tailing composite microcrystalline glass. The invention can prepare the iron tailing microcrystalline glass with good performance and white surface, overcomes the defects of the prior art and the current situation that the product color is single and difficult to adjust, and improves the color of the iron tailing microcrystalline glass, thereby expanding the application range of the iron tailing microcrystalline glass in building decoration materials, improving the utilization rate of iron tailings, realizing the purposes of saving resources, reducing production cost, protecting environment and the like.
Description
Technical Field
The invention relates to the technical field of microcrystalline glass, in particular to iron tailing composite microcrystalline glass and a preparation method thereof.
Background
The microcrystalline glass is widely applied to the fields of buildings, mechanical engineering, electronic industry, aerospace, national defense and military, biomedicine and the like due to the excellent performance of the microcrystalline glass. At present, the microcrystalline glass prepared by using the iron tailings is mainly researched in a laboratory, and a large-scale expansion test capable of industrial production is lacked. The process control and theoretical research of industrial production are incomplete, and the production cost cannot be effectively controlled. The fluctuation between the components of different types of iron tailings or the same type of iron tailings is large, which brings great difficulty to raw material selection and process manufacturing in actual production, so that the performance of the product is difficult to effectively control, and the product qualification rate is low. The microcrystalline glass prepared from the iron tailings mainly takes wollastonite or diopside as a main crystalline phase and takes the microcrystalline glass for buildings as a main crystalline phase. Because the iron tailings contain more kinds of coloring elements, the difficulty for removing the coloring elements is high, and the cost is high, the iron tailings microcrystalline glass has the advantages of dark color, high color adjustment difficulty and single color variety, thereby limiting the popularization and the application of the iron tailings microcrystalline glass.
Disclosure of Invention
In view of this, the embodiment of the invention provides the iron tailing composite glass ceramics and the preparation method thereof, wherein the iron tailing composite glass ceramics has good performance, white material surface and easily-adjustable color, and is suitable for industrial application.
The embodiment of the invention provides iron tailing composite glass ceramics, which comprises a base layer and a surface layer which are combined together, wherein the base layer contains iron tailing, the surface layer does not contain iron tailing, the crystal phase of the surface layer is different from that of the base layer, and the glass melting point of the surface layer is lower than that of the base layer.
Further, the substrate layer is prepared from the following raw materials in parts by weight: 30-40 parts of iron tailings, 14-20 parts of potassium feldspar, 6-7 parts of calcite, 35-45 parts of quartz powder and A12O34-7 parts of MgO 1-3 parts of B2O31 part of Sb2O31 part and 1-3 parts of ZnO.
Further, the surface layer is prepared from the following raw materials in parts by weight: 23-28 parts of potash feldspar, 14-18 parts of calcite, 40-50 parts of quartz powder and A12O36-8 parts of MgO 6-10 parts of B2O31 part of Sb2O31 part and 1-3 parts of ZnO.
A preparation method of iron tailing composite microcrystalline glass comprises the following steps:
s1, accurately weighing raw materials of a base layer and a surface layer respectively, and uniformly mixing the raw materials respectively;
s2, respectively carrying out vibration grinding until the granularity is below 200 meshes and the screen allowance is below 8%;
s3, respectively filling ground base layer powder and ground surface layer powder into a crucible;
s4, putting the crucible filled with the base layer powder and the surface layer powder into a high-temperature resistance furnace for melting;
s5, pouring the molten basal layer glass liquid and the molten surface layer glass liquid into water respectively for quenching;
s6, respectively putting the cooled substrate layer glass granules and the cooled surface layer glass granules into an electric heating forced air drying box for drying;
s7, vibrating and grinding the basal layer glass sample, and screening by using a 100-mesh sieve until all powder is smaller than 100 meshes for later use; vibrating and grinding the surface layer glass sample, sieving by using combined sieves of 40 meshes, 60 meshes, 100 meshes and 200 meshes, and circularly sieving for multiple times until the content of powder of-100 +200 meshes reaches more than 50% for later use;
s8, padding demoulding paper in the crucible, paving ground basal layer glass sample powder, paving ground surface layer glass sample powder, and paving;
s9, placing the crucible containing the powder in the step S8 into a high-temperature resistance furnace for heat treatment, and demolding to obtain the iron tailing composite microcrystalline glass.
Further, the vibration grinding is finished by a vibration sample grinding machine, and the vibration frequency of the vibration sample grinding machine is 710 r/min.
Further, in step S4, the melting temperature system is: the temperature was raised from room temperature to 1000 ℃ at a ramp rate of 5 ℃/min, then from 1000 ℃ to 1300 ℃ at a ramp rate of 2 ℃/min, then from 1300 ℃ to 1450 ℃ at a ramp rate of 1 ℃/min, and finally held at 1450 ℃ for two hours.
Further, in the step S6, the cooled base layer glass granules and the cooled surface layer glass granules are dried in an electric heating blowing dry box for 12 hours at a drying temperature of 70 ℃.
Further, in step S9, the heat treatment temperature profile is: raising the temperature from room temperature to 890 ℃ at the heating rate of 5 ℃/min, then preserving the heat at 890 ℃ for two hours, then raising the temperature from 890 ℃ to 1140 ℃ at the heating rate of 2 ℃/min, and finally preserving the heat at 1140 ℃ for half an hour.
Compared with the prior art, the invention has the following advantages: the color of the iron tailing microcrystalline glass can be improved, so that the application range of the iron tailing microcrystalline glass in building decoration materials is expanded, and the utilization rate of the iron tailings is improved. The iron tailing microcrystalline glass has the bending strength (32.5MPa) and the density (2.545 g-cm)-3) Good performances such as hardness (6-7), water absorption (0.036%), etc., and is superior to the industrial standard.
Drawings
Fig. 1 is a flow chart of a preparation method of the iron tailing composite glass ceramics.
FIG. 2 is a crystal phase result diagram of X-ray diffraction analysis of the iron tailing composite microcrystalline glass surface layer prepared under different crystallization temperature conditions.
FIG. 3 is a crystal phase result of X-ray diffraction analysis of the iron tailing composite microcrystalline glass substrate layer prepared under different crystallization temperature conditions.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, embodiments of the present invention will be further described with reference to the accompanying drawings.
The embodiment of the invention provides iron tailing composite glass ceramics, which comprises a base layer and a surface layer which are combined together, wherein the main influencing element causing the iron tailing glass ceramics to have dark color is iron, the base layer contains iron tailings, the surface layer does not contain the iron tailings, and the chemical components of the iron tailings are shown in Table 1. The granularity of the iron tailings, namely 100 meshes, is 70.77%, the iron tailings do not need to be crushed and ground separately in the process of preparing the glass ceramics, the energy consumption is greatly reduced, and the granularity composition of the iron tailings is shown in table 2.
TABLE 1
TABLE 2
The X-ray diffraction analysis result of the composite glass-ceramic shows that the crystal phase compositions of the surface layer and the substrate layer are different, as shown in fig. 2, the main crystal phases in the surface layer are diopside and albite, and fig. 3 shows that the main crystal phases in the substrate layer are diopside, albite and magnetite, but the crystal phase compositions of the substrate layer and the surface layer are not greatly different, so that the physical properties of the two layers are similar, and the interface of the composite glass-ceramic has good bonding property. The glass melting point of the surface layer is lower than that of the substrate layer, so that the surface layer can be uniformly paved on the substrate layer in the crystallization process, and the interface is bonded more tightly.
SiO2: as the main framework of the network structure of the glass ceramics, the structure of the glass ceramics is strengthened and the strength is increased with the increase of the addition amount in a certain range, and the melting point is increased when melting.
A12O3: all participate in a silica network structure by four coordination, the network structure of the glass is strengthened, the migration of mass points, especially alkali metal, in the glass at high temperature is limited, and the precipitated crystal phase is greatly influenced. The crystal content of the microcrystalline glass sample decreased with increasing alumina incorporation.
CaO: with CaO and SiO2The content ratio is increased, the glass transition temperature and the crystallization exothermic peak temperature are gradually reduced, and the crystallization exothermic peak becomes sharp. Increase CaO and SiO2The ratio lowers the devitrification activation energy and sintering temperature of the glass, but increases the dielectric constant, dielectric loss and thermal expansion coefficient of the sample.
MgO: in a certain range, as the addition amount of magnesium oxide is increased, the melting temperature of the microcrystalline glass is in a trend of decreasing, the viscosity is reduced, the speed is slowed down, and the forming is facilitated; and the crystallization performance of the microcrystalline glass can be enhanced, the content of a crystalline phase is increased, and the radius of a crystal grain is increased.
R2O: with the increase of the addition amount of the alkali metal, the nucleation temperature and the crystallization temperature of the glass ceramics are both lowered.
B2O3And Sb2O3: as a clarifying and whitening agent. Gases are excluded during the glass melting process.
ZnO and zinc oxide can reduce the melting temperature of the glass to a certain extent, along with the increase of the content of the zinc oxide, the crystallization of the system is easier,
Fe2O3: the addition of the iron oxide can make the crystallization of the microcrystalline glass easier and the crystal grains smaller, but the nucleation and crystallization temperature and the crystallization heat preservation time need to be strictly controlled, otherwise the defects of cracking, bubbles and the like of the sample are easily caused.
The iron tailings, potassium feldspar, calcite and quartz powder were subjected to chemical analysis, and their chemical compositions are shown in table 3.
Table 3 units of measurement: omega (B)/10-2
Therefore, the base layer is prepared from the following raw materials in parts by weight: 30-40 parts of iron tailings, 14-20 parts of potassium feldspar, 6-7 parts of calcite, 35-45 parts of quartz powder and A12O34-7 parts of MgO 1-3 parts of B2O31 part of Sb2O31 part and 1-3 parts of ZnO.
The surface layer is prepared from the following raw materials in parts by weight: 23-28 parts of potash feldspar, 14-18 parts of calcite, 40-50 parts of quartz powder and A12O36-8 parts of MgO 6-10 parts of B2O31 part of Sb2O31 part and 1-3 parts of ZnO.
Referring to fig. 1, a method for preparing iron tailing composite microcrystalline glass includes the following steps:
s1, accurately weighing raw materials of a base layer and a surface layer respectively, and uniformly mixing the raw materials respectively;
s2, respectively carrying out vibration grinding until the granularity is below 200 meshes, the screen allowance is below 8%, preferably finishing the vibration grinding through a vibration sample grinding machine, and preferably selecting the vibration frequency of the vibration sample grinding machine to be 710 r/min;
s3, respectively filling ground base layer powder and ground surface layer powder into a crucible;
s4, respectively putting the crucibles filled with the base layer powder and the surface layer powder into a high-temperature resistance furnace for melting, wherein the melting temperature system is as follows: raising the temperature from room temperature to 1000 ℃ at a temperature raising rate of 5 ℃/min, raising the temperature from 1000 ℃ to 1300 ℃ at a temperature raising rate of 2 ℃/min, raising the temperature from 1300 ℃ to 1450 ℃ at a temperature raising rate of 1 ℃/min, and finally preserving the temperature at 1450 ℃ for two hours;
s5, pouring the molten basal layer glass liquid and the molten surface layer glass liquid into water respectively for quenching;
s6, respectively putting the cooled substrate layer glass granules and the cooled surface layer glass granules into an electric heating forced air drying box, preferably keeping the temperature for 12 hours, and drying at the drying temperature of 70 ℃;
s7, vibrating and grinding the basal layer glass sample, and sieving the ground basal layer glass sample by using a 100-mesh sieve until the granularity of all powder is smaller than 100 meshes for later use; vibrating and grinding the surface layer glass sample, sieving by using combined sieves of 40 meshes, 60 meshes, 100 meshes and 200 meshes, and circularly sieving for multiple times until the content of powder of-100 +200 meshes reaches more than 50% for later use;
s8, padding demoulding paper in the crucible, paving ground basal layer glass sample powder, paving ground surface layer glass sample powder, and paving;
s9, placing the crucible containing the powder in the step S8 into a high-temperature resistance furnace for heat treatment, wherein the heat treatment temperature schedule is as follows: heating from room temperature to 890 ℃ at the heating rate of 5 ℃/min, then preserving heat at 890 ℃ for two hours, then heating from 890 ℃ to 1140 ℃ at the heating rate of 2 ℃/min, and finally preserving heat at 1140 ℃ for half an hour; and demolding to obtain the iron tailing composite microcrystalline glass.
Cutting the prepared microcrystalline glass test block by a cutting machine according to a certain size, grinding each surface of the cut microcrystalline glass to be smooth by a polishing machine, removing surface impurities, and preparing into a standard block shape.
Detailed description of the preferred embodiment 1
According to the experimental requirement, 1kg of samples are required to be respectively prepared for a base layer formula and a surface layer formula, and as the maximum material allowed to be put into a vibration sample grinding machine every time is 100g, the 1kg of samples are uniformly divided into 10 parts for preparation, and agglomeration and large blocks in raw materials are subjected to primary crushing.
Accurately weighing the raw materials according to the formula by using an electronic balance, filling the raw materials into a sample bag, uniformly mixing and numbering.
The operation process of the vibration sample grinding machine comprises the following steps: loading → turning on the power switch → timing → starting at 710r/min → grinding → turning off the power → sampling and cleaning.
In order to reduce melting temperature and save energy consumption before sample grinding, the granularity of a sample needs to be ground to be less than 200 meshes, and the sample granularity with different grinding time needs to be explored. Taking 100g of raw materials of a substrate layer and a surface layer respectively to carry out a grinding experiment, wherein the specific flow comprises the following steps: raw material → grinding → sieving → weighing.
And (3) putting each 100g of the weighed raw materials into a vibration sample grinder in sequence, grinding for 3min, taking out, and uniformly mixing the samples. The ground raw materials for the base layer and the surface layer were placed in 200ml crucibles, respectively, in preparation for melting the powder into glass.
Compacting the powder in the crucible, putting the crucible into a silicon-molybdenum rod high-temperature resistance furnace, turning on a power switch, setting a temperature schedule in a program, starting the program and turning on a working switch of the silicon-molybdenum rod high-temperature resistance furnace; and (3) 10 minutes before the melting procedure is finished, connecting half of the pot water by using a steel pot, carrying out thermal insulation gloves and sunglasses, closing a power switch when the procedure is finished, opening a furnace door, taking out the crucible by using iron tongs, and respectively pouring the basal layer glass liquid and the surface layer glass liquid in the crucible into the steel pot filled with water for quenching. And slowly pouring out water in the steel basin after cooling, then putting the cooled glass granules into an electric heating blowing drying box, keeping the temperature for 12 hours, and drying, wherein the set temperature is 70 ℃, so that the substrate layer glass granules and the surface layer glass granules are obtained.
Melting temperature system: the temperature was raised from room temperature to 1000 ℃ at a ramp rate of 5 ℃/min, then from 1000 ℃ to 1300 ℃ at a ramp rate of 2 ℃/min, then from 1300 ℃ to 1450 ℃ at a ramp rate of 1 ℃/min, and finally held at 1450 ℃ for two hours.
And (3) putting 100g of the dried basal layer glass sample into a vibration sample grinding machine each time, grinding for 10 seconds at 710r/min, sieving by using a 100-mesh sieve, putting glass powder with the size smaller than 100 meshes below the sieve into a marked sample bag, putting materials with the size larger than 100 meshes above the sieve into a grinding machine, grinding and sieving for multiple times for 10 seconds until all the powder is smaller than 100 meshes, and putting the materials into the sample bag for later use.
100g of surface layer glass sample is taken each time and put into a vibration sample grinder to be ground for 10 seconds at 710r/min, screening and grading are carried out by using combined screens of 40 meshes, 60 meshes, 100 meshes and 200 meshes, the powder is circularly screened for a plurality of times until the part of-100 +200 meshes reaches more than 50 percent, and the graded powder is respectively put into sample bags marked with-40 +60 meshes, -60+100 meshes, -100+200 meshes and-200 meshes for standby.
Taking a clean crucible, padding demoulding paper, firstly laying a layer of ground basal layer glass powder, then laying a layer of ground surface layer glass powder, laying the ground basal layer glass powder and the ground surface layer glass powder, putting the ground basal layer glass powder into a high-temperature resistance furnace after the ground basal layer glass powder is laid flat, closing a furnace door, opening a power switch, setting a temperature system in the program, starting the high-temperature resistance furnace, closing a power supply after the temperature in the furnace is reduced to room temperature, taking out fired microcrystalline glass, and putting the fired microcrystalline glass into a marked sample bag for storage.
Temperature system of crystallization process (taking 1140 ℃ as an example for setting crystallization temperature): raising the temperature from room temperature to 890 ℃ at the heating rate of 5 ℃/min, then preserving the heat at 890 ℃ for two hours, then raising the temperature from 890 ℃ to 1140 ℃ at the heating rate of 2 ℃/min, and finally preserving the heat at 1140 ℃ for half an hour.
Cutting the prepared microcrystalline glass test block by a cutting machine according to a certain size, grinding each surface of the cut microcrystalline glass to be smooth by a polishing machine, removing surface impurities, and preparing into a standard block shape. Placing into a marked sample bag.
The results of the physical and chemical property tests of the iron tailing microcrystalline glass and the comparison with the industry standard are shown in table 4.
TABLE 4
As can be seen from Table 4, the prepared microcrystalline glass has bending strength and Mohs hardness superior to those of JC/T872-2000 microcrystalline glass for architectural decoration, and has lower density and water absorption.
The invention can improve the color of the iron tailing microcrystalline glass, thereby expanding the application range of the iron tailing microcrystalline glass in building decoration materials, improving the utilization rate of the iron tailings, and having good performance which is superior to the industrial standard.
The features of the embodiments and embodiments described herein above may be combined with each other without conflict.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (8)
1. The composite microcrystalline glass with the iron tailings is characterized by comprising a substrate layer and a surface layer which are combined together, wherein the substrate layer contains the iron tailings, the surface layer does not contain the iron tailings, the crystal phase of the surface layer is different from that of the substrate layer, the main crystal phases of the surface layer are diopside and albite, the main crystal phases of the substrate layer are diopside, albite and magnetite, and the surface layer is white; the glass melting point of the surface layer is lower than that of the substrate layer; the iron tailings comprise the following components in percentage by mass: 30.26% SiO2、17.01％TFe2O3、16.55％MgO、13.16％CaO、5.01％Al2O3、1.10％K2O、0.42％Na2O, loss on ignition 15.42% and other 2.52%.
2. The iron tailing composite glass ceramic according to claim 1, wherein the substrate layer is prepared from the following raw materials in parts by weight: 30-40 parts of iron tailings, 14-20 parts of potassium feldspar, 6-7 parts of calcite, 35-45 parts of quartz powder and A12O34-7 parts of MgO 1-3 parts of B2O31 part of Sb2O31 part and 1-3 parts of ZnO.
3. The iron tailing composite glass ceramic according to claim 1, wherein the surface layer is prepared from the following raw materials in parts by weight: 23-28 parts of potash feldspar, 14-18 parts of calcite, 40-50 parts of quartz powder and A12O36-8 parts of MgO 6-10 parts of B2O31 part of Sb2O31 part, 1-3 parts of ZnO; the potassium feldspar comprises the following chemical components in percentage by weight: 64.57% SiO2、0.29％TFe2O3、0.04％MgO、0.16％CaO、18.88％Al2O3、12.81％K2O、2.46％Na2O, loss on ignition 0.26% and others 0.07%; the calcite comprises the following chemical components in percentage by weight: 0.1% SiO2、0％TFe2O3、0.36％MgO、55.49％CaO、0.24％Al2O3、0.01％K2O、0.07％Na2O, loss on ignition 43.44% and other 0.08%; the quartz powder comprises the following chemical components in percentage by weight: 99.54% SiO2、0.02％TFe2O3、0.01％MgO、0.03％CaO、0.01％Al2O3、0％K2O、0％Na2O, loss on ignition 0.22% and others 0.07%.
4. The preparation method of the iron tailing composite glass ceramic as defined in any one of claims 1 to 3, which comprises the following steps:
s1, accurately weighing raw materials of a base layer and a surface layer respectively, and uniformly mixing the raw materials respectively;
s2, respectively carrying out vibration grinding until the granularity is below 200 meshes and the screen allowance is below 8%;
s3, respectively filling ground base layer powder and ground surface layer powder into a crucible;
s4, putting the crucible filled with the base layer powder and the surface layer powder into a high-temperature resistance furnace for melting;
s5, pouring the molten basal layer glass liquid and the molten surface layer glass liquid into water respectively for quenching;
s6, respectively putting the cooled substrate layer glass granules and the cooled surface layer glass granules into an electric heating forced air drying box for drying;
s7, vibrating and grinding the basal layer glass sample, and screening by using a 100-mesh sieve until all powder is smaller than 100 meshes for later use; vibrating and grinding the surface layer glass sample, sieving by using combined sieves of 40 meshes, 60 meshes, 100 meshes and 200 meshes, and circularly sieving for multiple times until the content of powder of-100 +200 meshes reaches more than 50% for later use;
s8, padding demoulding paper in the crucible, paving ground basal layer glass sample powder, paving ground surface layer glass sample powder, and paving;
s9, placing the crucible containing the powder in the step S8 into a high-temperature resistance furnace for heat treatment, and demolding to obtain the iron tailing composite microcrystalline glass.
5. The preparation method of the iron tailing composite microcrystalline glass according to claim 4, wherein the vibration grinding is completed through a vibration sample grinding machine, and the vibration frequency of the vibration sample grinding machine is 710 r/min.
6. The method for preparing the iron tailing composite glass ceramic according to claim 4, wherein in the step S4, the melting temperature system is as follows: the temperature was raised from room temperature to 1000 ℃ at a ramp rate of 5 ℃/min, then from 1000 ℃ to 1300 ℃ at a ramp rate of 2 ℃/min, then from 1300 ℃ to 1450 ℃ at a ramp rate of 1 ℃/min, and finally held at 1450 ℃ for two hours.
7. The method for preparing the iron tailing composite glass-ceramic according to claim 4, wherein in the step S6, the cooled base layer glass granules and the cooled surface layer glass granules are dried in an electrothermal blowing drying oven for 12 hours at a drying temperature of 70 ℃.
8. The method for preparing the iron tailing composite glass ceramic according to claim 4, wherein in the step S9, the heat treatment temperature schedule is as follows: raising the temperature from room temperature to 890 ℃ at the heating rate of 5 ℃/min, then preserving the heat at 890 ℃ for two hours, then raising the temperature from 890 ℃ to 1140 ℃ at the heating rate of 2 ℃/min, and finally preserving the heat at 1140 ℃ for half an hour.
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Effective date of registration: 20220509 Address after: 034000 Yangmingbao Town Industrial Park, Dai County, Xinzhou City, Shanxi Province Patentee after: Shanxi Boyuan microcrystalline Co.,Ltd. Address before: 321000 No. 1188, Huafeng West Road, Jindong Economic Development Zone, Jinhua City, Zhejiang Province (shoe pond exit of Hangzhou Jinqu Expressway) Patentee before: Zhejiang Jinxiu Nanguo Technology Co.,Ltd. Effective date of registration: 20220509 Address after: 321000 No. 1188, Huafeng West Road, Jindong Economic Development Zone, Jinhua City, Zhejiang Province (shoe pond exit of Hangzhou Jinqu Expressway) Patentee after: Zhejiang Jinxiu Nanguo Technology Co.,Ltd. Address before: 430074 No. 388 Lu Lu, Hongshan District, Hubei, Wuhan Patentee before: CHINA University OF GEOSCIENCES (WUHAN CITY) |
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