Industrial microcrystalline plate manufactured from graphite tailings and manufacturing method of industrial microcrystalline plate

Abstract

The invention relates to the technical field of microcrystalline plates, in particular to an industrial microcrystalline plate manufactured from graphite tailings and a manufacturing method, the industrial microcrystalline plate is prepared from the following raw material components in percentage by mass: 62-70% of graphite tailings, 6-10% of quartz sand, 6.0-7.0% of sodium carbonate, 5-7% of limestone, 2-2.8% of dolomite, 3-4% of sodium fluosilicate, 1.5-2% of sodium nitrate and 0.1-0.2% of cerium oxide. By analyzing the components of the graphite tailings and adopting a specific formula combination, the graphite tailings are manufactured into the microcrystalline plate with excellent industrial wear resistance and corrosion resistance, so that the problems that the microcrystalline plate manufactured by the existing formula is poor in wear resistance and poor in corrosion resistance are solved. The wear-resistant lining is not applicable to gangue bins, coal storage bunkers, dumper rooms and coal preparation plant equipment in the coal industry.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of microcrystalline board, and particularly relates to a graphite tailings manufacturing industrial microcrystalline board and a manufacturing method. BACKGROUND

[0002] The graphite tailings have a large stock, occupy a large amount of land resources for stacking, pollute the environment, and the national solid waste resource requirement is developed around the core principles of reduction, resource, and harmlessness, which is embodied in multiple aspects. In the aspects of technical research and application, breakthroughs in key technologies for solid waste resource utilization are emphasized, such as gradient high-quality utilization, valuable component extraction, and coupled high-value utilization, and the research and development and integrated demonstration of large-scale utilization complete technology are promoted.

[0003] The patent document with the patent number CN119912161A discloses a microcrystalline board based on hazardous waste incineration ash production, which comprises fly ash, bottom ash, silica sand, anhydrous sodium carbonate, sodium nitrate, anhydrous potassium carbonate, sodium fluorosilicate, tin dioxide, nickel oxide, cobalt oxide, anhydrous borax, cerium dioxide, manganese dioxide, and lanthanum oxide.

[0004] However, in the actual use process, the inventors found that the microcrystalline board made of the existing formula has poor wear resistance, and is not suitable for application in the wear-resistant lining of the gangue warehouse, coal storage warehouse, tippler room, and coal preparation plant equipment in the coal industry. SUMMARY

[0005] The purpose of the present application is to solve the technical problems of the existing formula for making microcrystalline board with poor wear resistance, which is not suitable for application in the wear-resistant lining of the gangue warehouse, coal storage warehouse, tippler room, and coal preparation plant equipment in the coal industry, by analyzing the composition of graphite tailings, using a specific formula combination, and making industrial microcrystalline board with superior wear-resistant and corrosion-resistant performance.

[0006] To solve the above technical problems, the technical scheme is as follows: A graphite tailings manufacturing industrial microcrystalline board, the raw material components are as follows in percentage by mass: The graphite tailings are 62-70%, the quartz sand is 6-10%, the soda ash is 6.0-7.0%, the limestone is 5-7%, the dolomite is 2-2.8%, the sodium fluorosilicate is 3-4%, the sodium nitrate is 1.5-2%, and the cerium oxide is 0.1-0.2%.

[0007] As a preferred, the raw material components are as follows in percentage by mass: The graphite tailings are 70%, the quartz sand is 10%, the soda ash is 6.0%, the limestone is 5%, the dolomite is 2.8%, the sodium fluorosilicate is 4%, the sodium nitrate is 2%, and the cerium oxide is 0.2%.

[0008] As preferred, the raw material components include the following oxides in mass percentage: SiO2 is 40-60%, Al2O3 is 5-10%, Fe2O3 < 5%, CaO is 10-20%, MgO is 3-10%, K2O+Na2O is 5-10%, and F is 1.5-3%.

[0009] As preferred, the graphite tailings have a particle size of ≥60 mesh and include the following oxides in mass percentage: SiO2 is 45-75%, Al2O3 is 6-13%, Fe2O3 < 9%, CaO is 6-11%, MgO is 4-9%, K2O+Na2O is 4-11%, and F is 1.4-2.9%.

[0010] As preferred, the quartz sand has a particle size of ≥20 mesh and includes the following oxides in mass percentage: SiO2 is 35-65%, Al2O3 is 4-9%, Fe2O3 < 8%, CaO is 4-11%, MgO is 2-8%, K2O+Na2O is 3-10%, and F is 1.3-2.8%.

[0011] As preferred, the limestone has a particle size of ≥20 mesh and includes the following oxides in mass percentage: SiO2 is 50-70%, Al2O3 is 7-15%, Fe2O3 < 7%, CaO is 5-10%, MgO is 5-10%, K2O+Na2O is 3-9%, and F is 1.2-2.7%.

[0012] As preferred, the dolomite has a particle size of ≥20 mesh and includes the following oxides in mass percentage: SiO2 is 20-55%, Al2O3 is 8-15%, Fe2O3 < 6%, CaO is 5-15%, MgO is 6-11%, K2O+Na2O is 2-8%, and F is 1.0-2.5%.

[0013] As further preferred, the soda ash, sodium fluosilicate, sodium nitrate and cerium oxide are of chemical grade purity.

[0014] The present application also provides a method for manufacturing microcrystalline plate, which is applied to manufacturing the above-mentioned graphite tailings into industrial microcrystalline plate, and includes the following steps: Step one, raw material mixing, the raw materials are weighed according to the proportion, mixed in the mixer, and 3-5% water is added to the total weight of the mixture, mixed for 3-5 minutes, and then sent to the full-electricity melting furnace feeding bin; Step two, melting of the mixture, using an automatic feeder to feed and through an infrared liquid level instrument to control the feeding; the mixture is melted, clarified and homogenized in a main melting tank, and is maintained for about 8 hours, the melting temperature of the mixture is 1400-1500 DEG C, the clarification and homogenization temperature is 1450-1520 DEG C; the clarified and homogenized glass enters a material channel through a flow liquid hole and an ascending channel, the temperature is controlled at 1250-1300 DEG C, after cooling through the material channel, the glass enters a calender to be calendered and formed, the forming temperature is 1050-1150 DEG C; Step three, calendering and forming, two glass calenders are used for calendering and forming in each production line, the thickness and width of the plate are adjusted according to the production requirements, the formed glass band enters an annealing kiln through a conveying roller way for annealing; Step four, annealing, the glass band enters the annealing kiln at a temperature of 600-750 DEG C, after being kept at 600-700 DEG C for 10-20 minutes, the temperature is decreased to 520-600 DEG C at a speed of 3-5 DEG C / min, then decreased to 300 DEG C at a speed of 7-12 DEG C / min, and cooled to 40 DEG C after 40-60 minutes to exit the kiln, and then enters a cold end cutting process; the cold end cutting process cuts the glass band to form an annealed plate as a semi-finished product, which is sent to a crystallization kiln through a transition roller table for crystallization; Step five, crystallization, the annealed plate that passes the detection enters the crystallization kiln, is heated to 650-710 DEG C for 30-90 minutes, is kept at 650-710 DEG C for 30-90 minutes for nucleation, is heated to 900-950 DEG C for 30-120 minutes for crystallization, and is cooled to 40 DEG C after 60-120 minutes to exit the kiln, thus completing the crystallization process and becoming a crystallized plate.

[0015] As a further optimization, the crystallized plate obtained in the step five has a bending strength ≥100 MPa, a compressive strength ≥900 MPa, and an abrasion loss ≤0.02 g / cm 2 .

[0016] The beneficial effects of the present application are: (1) In the present application, through analysis of the composition of graphite tailings, slag resources are reasonably utilized, high-value-added microcrystalline glass decorative materials are researched and developed, which has important significance for saving energy, turning waste into treasure, improving the environment, and improving economic and social benefits. At the same time, the product is measured, has superior wear-resistant and corrosion-resistant performance, meets the industrial microcrystalline plate standard, and can be widely used in the steel, coal, electric power and chemical industry; (3) In this invention, ferric oxide is used as the main nucleating agent and fluoride is used as the nucleation inducing agent to accelerate the nucleation and crystallization process. Due to the high iron content, the melting thermal conductivity is poor during the preparation of microcrystalline glass. All-electric melting or electric-assisted melting is adopted to make the mixture generate its own heat. Under the action of the three fields of thermal field, current field and glass fluid flow field, the melting homogeneity is promoted, ensuring the feasibility of production and laying a theoretical and practical foundation for stable production and high product qualification rate.

[0017] In summary, this product has the advantages of high wear resistance and excellent corrosion resistance, and is especially suitable for the field of microcrystalline board technology. Attached Figure Description

[0018] To more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings used in the description of the embodiments will be briefly introduced below. Obviously, the drawings described below are only some embodiments of the present invention. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.

[0019] Figure 1 Add photos to the product. Detailed Implementation

[0020] The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings.

[0021] Example 1 like Figure 1 As shown, a type of industrial microcrystalline sheet made from graphite tailings has the following raw material components by mass percentage: The composition of the material is as follows: graphite tailings 62-70%, quartz sand 6-10%, soda ash 6.0-7.0%, limestone 5-7%, dolomite 2-2.8%, sodium fluorosilicate 3-4%, sodium nitrate 1.5-2%, and cerium oxide 0.1-0.2%.

[0022] Furthermore, the raw material components, by mass percentage, are as follows: The composition is 70% graphite tailings, 10% quartz sand, 6.0% soda ash, 5% limestone, 2.8% dolomite, 4% sodium fluorosilicate, 2% sodium nitrate, and 0.2% cerium oxide.

[0023] Cerium oxide, as a rare earth additive, refines grains and fills micropores in the glass phase, thereby increasing the density of the material and directly enhancing its wear resistance.

[0024] Furthermore, sodium fluorosilicate, as a key nucleating agent, promotes the directional growth of wollastonite crystals by regulating the release rate of F⁻ ions, thereby enhancing crystal quality. At the same time, sodium fluorosilicate replaces traditional fluorite (CaF₂), avoiding fluorine volatilization pollution.

[0025] Further, the graphite tailings utilization rate in the embodiment reaches 70%, reducing the pollution of stacking, and greatly reducing the raw material cost compared with pure sand-based plate materials.

[0026] Further, the raw material components include the following oxides in mass percentage: SiO2 is 40-60%, Al2O3 is 5-10%, Fe2O3 < 5%, CaO is 10-20%, MgO is 3-10%, K2O+Na2O is 5-10%, and F is 1.5-3%.

[0027] It should be noted that by limiting the oxide content of the raw material, the balance between the melt viscosity and the crystallization kinetics is ensured, avoiding brittle fracture caused by excessive crystal growth.

[0028] Further, the graphite tailings particle size is ≥60 mesh, which includes the following oxides in mass percentage: SiO2 is 45-75%, Al2O3 is 6-13%, Fe2O3 < 9%, CaO is 6-11%, MgO is 4-9%, K2O+Na2O is 4-11%, and F is 1.4-2.9%. Further, the quartz sand particle size is ≥20 mesh, which includes the following oxides in mass percentage: SiO2 is 35-65%, Al2O3 is 4-9%, Fe2O3 < 8%, CaO is 4-11%, MgO is 2-8%, K2O+Na2O is 3-10%, and F is 1.3-2.8%. Further, the limestone particle size is ≥20 mesh, which includes the following oxides in mass percentage: SiO2 is 50-70%, Al2O3 is 7-15%, Fe2O3 < 7%, CaO is 5-10%, MgO is 5-10%, K2O+Na2O is 3-9%, and F is 1.2-2.7%. Further, the dolomite particle size is ≥20 mesh, which includes the following oxides in mass percentage: SiO2 is 20-55%, Al2O3 is 8-15%, Fe2O3 < 6%, CaO is 5-15%, MgO is 6-11%, K2O+Na2O is 2-8%, and F is 1.0-2.5%. Further, the sodium fluoride, sodium fluoride, sodium nitrate, and cerium oxide are of chemical purity.

[0029] Example 1 A graphite tailings manufacturing industrial microcrystalline plate material, the raw material components include the following oxides in mass percentage: SiO2 is 60%, Al2O3 is 8%, Fe2O3 is 2.5%, CaO is 12%, MgO is 8%, K2O+Na2O is 8%, and F is 1.5%.

[0030] Example 2 The graphite tailings manufacturing industrial microcrystalline board material, raw material components include the following by mass percent of each oxide: SiO2 is 60%, Al2O3 is 7.5%, Fe2O3 is 2.5%, CaO is 12%, MgO is 8%, K2O+Na2O is 8%, F is 2.0%.

[0031] Example 3 The graphite tailings manufacturing industrial microcrystalline board material, raw material components include the following by mass percent of each oxide: SiO2 is 60%, Al2O3 is 7%, Fe2O3 is 2.5%, CaO is 12%, MgO is 8%, K2O+Na2O is 8%, F is 2.5%.

[0032] The performance indicators of the microcrystalline industrial board material made based on the formulations of examples 1-3 are shown in Table 1: Table 1

[0033] It can be seen that the change of fluorine content has a greater impact on the performance of the product, because the microstructure of the microcrystalline material is a mixture of crystals and glass, and appropriate fluorine content helps the growth of crystals, the proportion of crystals is high, and the content of glass is low, the product has good wear resistance and corrosion resistance. When the fluorine content is too high or too low, it will affect the growth of crystals, and the product performance will appear problems such as not wear-resistant or low strength. Specifically, insufficient fluorine leads to a small number of crystal nuclei and a high proportion of glass phase, resulting in poor wear resistance, while excessive fluorine causes rapid crystal growth, producing stress microcracks. When the fluorine content is optimal, the crystal interlocking structure is complete and the glass phase is dense, therefore the introduction and retention rate of fluorine is also the focus of this technology.

[0034] Comparative example The ordinary cast stone uses single basalt as raw material, while the graphite tailings manufacturing industrial microcrystalline board material in the present embodiment, the raw material components are as follows by mass percent: Graphite tailings 62-70%, quartz sand 6-10%, soda ash 6.0-7.0%, limestone 5-7%, dolomite 2-2.8%, sodium fluorosilicate 3-4%, sodium nitrate 1.5-2%, and cerium oxide 0.1-0.2%.

[0035] Table 2

[0036] According to the experimental results in the above table, compared with ordinary cast stone, the wear amount of the microcrystalline industrial board material in the present application is reduced by 60%, the sulfuric acid corrosion resistance is increased by 3.6%, and the compressive strength is increased by 53%.

[0037] Example two Wherein the same or corresponding parts as in example one with the corresponding reference numerals of example one, for the sake of simplicity, only the difference with example one is described below. The difference between this embodiment two and example one is: A method for manufacturing microcrystalline plate, using the graphite tailings manufacturing industry microcrystalline plate described in embodiment one, comprising the following steps: Step one, raw material mixing, the raw materials are weighed according to the proportion, mixed in the mixer, and 3-5% of the total weight of the mixture is added, mixed for 3-5 minutes, and then sent to the full electric melting furnace feeding bin; Step two, melting of the mixture, using automatic feeder to add material, and controlling the feeding through infrared liquid level instrument; The mixed material is melted, clarified and homogenized in the main melting pool, and the temperature is maintained at about 8 hours, the melting temperature of the mixed material is 1400-1500℃, the clarification and homogenization temperature is 1450-1520℃; The clarified and homogenized glass enters the material channel through the flow liquid hole and the riser, and the temperature is controlled at 1250-1300℃, after cooling through the material channel, it enters the calender to form a shape, and the forming temperature is 1050-1150℃; Step three, calendering, two glass calenders are used for calendering on each production line, the thickness and width of the plate are adjusted according to the production requirements, and the formed glass strip enters the annealing furnace after the conveying roller; Step four, annealing, the glass strip enters the annealing furnace at a temperature of 600-750℃, and after holding at 600-700℃ for 10-20 minutes, it is cooled at a speed of 3-5℃ / min to 520-600℃, and then at a speed of 7-12℃ / min to 300℃, and then cooled to 40℃ after 40-60 minutes to exit the furnace, and then enters the cold end cutting process; The cold end cutting process cuts the glass strip, and the cut glass strip forms a semi-finished product annealing plate, which is sent to the crystallization kiln through the transition roller table; Step five, crystallization, the qualified annealing plate enters the crystallization kiln, and is heated to 650-710℃ for 30-90 minutes, held at 650-710℃ for 30-90 minutes, and then heated to 900-950℃ for 30-120 minutes, held at 900-950℃ for 30-120 minutes, and then cooled to 40℃ after 60-120 minutes to exit the furnace, completing the crystallization process and becoming a crystallized plate.

[0038] It is worth noting that the nucleation stage adopts 650-710℃ for 30-90 minutes, which makes the crystal nucleus uniformly distributed and avoids local aggregation; The crystallization stage adopts 900-950℃ for 30-120 minutes, which accelerates the crystal growth and forms an interlocking structure, and the compressive strength is ≥900MPa.

[0039] Gradient annealing technology was also adopted, using a three-stage cooling rate from 3-5℃ / min to 7-12℃ / min, and finally natural cooling, which effectively eliminated residual stress in the glass phase, reduced microcracks, and made the bending strength ≥100MPa.

[0040] In the description of this invention, it should be understood that the terms "front and back", "left and right", etc., indicate the orientation or positional relationship based on the orientation or positional relationship shown in the accompanying drawings. They are only for the convenience of describing this invention and simplifying the description, and do not indicate or imply that the device or component referred to must have a specific orientation, or be constructed and operated in a specific orientation. Therefore, they should not be construed as limitations on the invention.

[0041] Of course, those skilled in the art should understand that the term "a" should be understood as "at least one" or "one or more". That is, in one embodiment, the number of an element can be one, while in another embodiment, the number of the element can be multiple. The term "a" should not be understood as a limitation on the quantity.

[0042] The above description is merely a preferred embodiment of the present invention, but the scope of protection of the present invention is not limited thereto. Any variations or substitutions that can be easily conceived by those skilled in the art under the technical guidance of the present invention should be included within the scope of protection of the present invention. Therefore, the scope of protection of the present invention should be determined by the scope of the claims.

Claims

1. An industrial micacrystalline board made of graphite tailings, characterized by, The raw material components are as follows in percentage by mass: The graphite tailings are 62-70%, the quartz sand is 6-10%, the soda ash is 6.0-7.0%, the limestone is 5-7%, the dolomite is 2-2.8%, the sodium fluosilicate is 3-4%, the sodium nitrate is 1.5-2%, and the cerium oxide is 0.1-0.2%.

2. A graphite tailings manufactured industrial microcrystalline board material according to claim 1, characterized by, The raw material components are as follows in percentage by mass: The graphite tailings are 70%, the quartz sand is 10%, the soda ash is 6.0%, the limestone is 5%, the dolomite is 2.8%, the sodium fluosilicate is 4%, the sodium nitrate is 2%, and the cerium oxide is 0.2%.

3. A graphite tailings manufactured industrial microcrystalline board material according to claim 1, characterized by, The raw material components include the following oxides in percentage by mass: SiO2 is 40-60%, Al2O3 is 5-10%, Fe2O3 < 5%, CaO is 10-20%, MgO is 3-10%, K2O+Na2O is 5-10%, and F is 1.5-3%.

4. A graphite tailings manufactured industrial microcrystalline board material according to claim 1, characterized by, The graphite tailings have a particle size of ≥60 mesh and include the following oxides in percentage by mass: SiO2 is 45-75%, Al2O3 is 6-13%, Fe2O3 < 9%, CaO is 6-11%, MgO is 4-9%, K2O+Na2O is 4-11%, and F is 1.4-2.9%.

5. A graphite tailings manufactured industrial microcrystalline board material according to claim 1, characterized by, The quartz sand has a particle size of ≥20 mesh and includes the following oxides in percentage by mass: SiO2 is 35-65%, Al2O3 is 4-9%, Fe2O3 < 8%, CaO is 4-11%, MgO is 2-8%, K2O+Na2O is 3-10%, and F is 1.3-2.8%.

6. A graphite tailings manufactured industrial microcrystalline board material according to claim 1, characterized by, The limestone has a particle size of ≥20 mesh and includes the following oxides in percentage by mass: SiO2 is 50-70%, Al2O3 is 7-15%, Fe2O3 < 7%, CaO is 5-10%, MgO is 5-10%, K2O+Na2O is 3-9%, and F is 1.2-2.7%.

7. A graphite tailings manufactured industrial microcrystalline board material according to claim 1, characterized by, The dolomite has a particle size of ≥20 mesh and includes the following oxides in percentage by mass: SiO2 is 20-55%, Al2O3 is 8-15%, Fe2O3 < 6%, CaO is 5-15%, MgO is 6-11%, K2O+Na2O is 2-8%, and F is 1.0-2.5%.

8. A graphite tailings manufactured industrial microcrystalline board material according to claim 1, characterized by, The soda ash, the sodium fluosilicate, the sodium nitrate, and the cerium oxide are of chemical purity.

9. A method for manufacturing microcrystalline board, applied to the manufacture of industrial microcrystalline board from graphite tailings according to any one of claims 1 to 8, characterized in that, The method includes the following steps: Step one, raw material mixing, the raw materials are weighed according to the proportion, mixed in the mixer, and 3-5% water of the total weight of the mixture is added, mixed for 3-5 minutes, and then sent to the full electric melting furnace feeding bin; Step two, melting of the mixture, automatic feeding machine is used for feeding, and the infrared liquid level instrument is used for controlling feeding; the mixture is melted, clarified, and homogenized in the main melting pool, and the temperature is maintained at about 8 hours, the melting temperature of the mixture is 1400-1500℃, the clarification and homogenization temperature is 1450-1520℃; the clarified and homogenized glass enters the material channel through the flow liquid hole and the rising channel, the temperature is controlled at 1250-1300℃, and after temperature reduction through the material channel, the glass enters the calendering machine for calendering and forming, the forming temperature is 1050-1150℃; Step three, calendering, two glass calendering machines are used in each production line for calendering, the thickness and width of the glass sheet are adjusted according to the production requirements, the formed glass ribbon enters the annealing lehr for annealing through the conveying roller table; Step four, annealing, the glass ribbon enters the annealing lehr at a temperature of 600-750 ℃, after being kept at 600-700 ℃ for 10-20 minutes, the temperature is decreased to 520-600 ℃ at a speed of 3-5 ℃ / min, then decreased to 300 ℃ at a speed of 7-12 ℃ / min, and then cooled to 40 ℃ after 40-60 minutes to exit the lehr, and then enters the cold end cutting process; the cold end cutting process cuts the glass ribbon, and the cut glass ribbon forms the semi-finished product annealed sheet, which is sent to the crystallization lehr for crystallization through the transition roller table; Step five, crystallization, the qualified annealed sheet enters the crystallization lehr, heated to 650-710 ℃ for 30-90 minutes, nucleated at 650-710 ℃ for 30-90 minutes, then heated to 900-950 ℃ for 30-120 minutes, crystallized at 900-950 ℃ for 30-120 minutes, cooled to 40 ℃ for 60-120 minutes to exit the lehr, and the crystallization process is completed to become the crystallized sheet.

10. A method for manufacturing a microcrystalline substrate according to claim 9, characterized in that, The step five obtains the crystallized plate with bending strength ≥ 100 MPa, compressive strength ≥ 900 MPa, and abrasion loss ≤ 0.02 g / cm 2 .

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