CN114538951A - Graphite multi-source solid waste-based foamed ceramic material, preparation method thereof and partition board - Google Patents

Graphite multi-source solid waste-based foamed ceramic material, preparation method thereof and partition board Download PDF

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CN114538951A
CN114538951A CN202210304115.4A CN202210304115A CN114538951A CN 114538951 A CN114538951 A CN 114538951A CN 202210304115 A CN202210304115 A CN 202210304115A CN 114538951 A CN114538951 A CN 114538951A
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graphite
foamed ceramic
ceramic material
solid waste
tailings
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CN114538951B (en
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胡锐
张韬
程飞飞
孔建军
顾锡丽
韦凯
赖玮
潘卫
张明
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Suzhou Sinoma Design And Research Institute Of Non Metallic Minerals Industry Co ltd
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    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
    • C04B38/02—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by adding chemical blowing agents
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B33/00—Clay-wares
    • C04B33/02—Preparing or treating the raw materials individually or as batches
    • C04B33/13—Compounding ingredients
    • C04B33/132—Waste materials; Refuse; Residues
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/74—Physical characteristics
    • C04B2235/77—Density
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P40/00—Technologies relating to the processing of minerals
    • Y02P40/60—Production of ceramic materials or ceramic elements, e.g. substitution of clay or shale by alternative raw materials, e.g. ashes

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Structural Engineering (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Environmental & Geological Engineering (AREA)
  • Dispersion Chemistry (AREA)
  • Compositions Of Oxide Ceramics (AREA)
  • Processing Of Solid Wastes (AREA)
  • Porous Artificial Stone Or Porous Ceramic Products (AREA)

Abstract

The invention discloses a graphite-based multi-source solid waste-based foamed ceramic material, a preparation method thereof and a partition board, wherein the foamed ceramic material comprises, by mass, 50-70% of graphite ore dressing tailings, 5-20% of mining waste rocks, 5-25% of exfoliated clay and 0-15% of auxiliary binder. By adopting the technical scheme of the invention, the graphite mining and selecting solid waste such as the exfoliated clay, the mining waste rock, the mineral processing tailings and the like is systematically utilized, three poor-quality resources of the graphite tailings are comprehensively utilized according to the proportioning design, no high-quality mineral resources are required to be added, the degree of dependence on external high-quality clay resources such as kaolin, feldspar and the like is greatly saved, the problem of mechanical property reduction of foamed ceramics caused by excessively high addition of the poor-quality mineral resources in the prior art is solved, the comprehensive utilization of the graphite multi-source solid waste is realized, the production cost is reduced, meanwhile, the consumption conveying of batch poor-quality solid waste to the building industry is realized, and the virtuous cycle of graphite mineral mining is promoted.

Description

Graphite multi-source solid waste-based foamed ceramic material, preparation method thereof and partition board
Technical Field
The invention relates to the technical field of new building materials, in particular to a graphite-based multi-source solid waste foamed ceramic material, a preparation method thereof and a partition board.
Background
Graphite can produce a large amount of solid wastes in the process of picking, wherein the peeled clay, the mined barren rocks and the mineral dressing tailings are the three largest types of solid wastes, and the stock of the graphite picking solid wastes in China currently exceeds 3 hundred million tons. According to the conventional stripping ratio of 3:1 and the estimation of 6-8% of fixed carbon content, more than 15 tons of picking solid waste can be generated every 1 ton of fine graphite powder, more than 1500 ten thousand tons of picking solid waste are generated every year in the graphite industry in recent years, and the speed is still increased every year along with the increase of the graphite demand. Development and utilization of bulk graphite mining and dressing solid wastes such as stripped clay, mining waste rock, mineral dressing tailings and the like are imperative.
At present, the main utilization directions of the graphite mining and selecting solid wastes comprise the recovery of valuable minerals, the preparation of white carbon black and the application in building material industry. Both the former two can not consume solid wastes in large quantities, so the application in the building material industry becomes an effective way for eliminating the solid wastes in the graphite picking. Generally, the mining waste rock is added in a proportion of 5-10% to be used in products with relatively low mechanical property requirements such as baking-free bricks, and the quality of the products is not met by adding a large amount of the mining waste rock.
On the other hand, the foamed ceramic material is a novel material developed in recent years, and has the advantages of high porosity, low thermal conductivity, light weight, high hardness, thermal shock resistance, high temperature resistance, corrosion resistance, good mechanical strength and the like. The foamed ceramic plate has the characteristics of light weight, good waterproofness, fire resistance, flame retardance, small deformation coefficient, aging resistance, stable performance and the like, has good compatibility with a wall base layer and a finishing layer, is safe and stable, and can overcome the defects of open fire resistance, easy aging and the like of organic materials. However, most of the existing foamed ceramic plates adopt expensive ores and fine ceramics as main raw materials, and have high production cost and consume a large amount of resources.
At present, the mineral tailings in solid waste are selected by using graphite to prepare the foamed ceramic material, for example, chinese invention patent CN101913899A discloses a method for preparing a coal gangue perforated brick by using high-calcium graphite mill tailings as a filler, the graphite mill tailings with high content of CaO is used as the filler, the coal gangue perforated brick is prepared with the addition of 30%, and the problem that CaO can not be used for producing a wall material due to water-powder brick bubbling in the perforated brick is solved by using the principle that the coal gangue and CaO generate calcium silicate in the high-temperature sintering process.
The Chinese invention patent CN112321319A discloses a foamed ceramic based on graphite tailings and a preparation method thereof, wherein the foamed ceramic comprises 45-70% of graphite tailings, 10-15% of quartz, 5-15% of bauxite and 15-25% of feldspar; simultaneously adding 0.1-0.5% of silicon carbide; the material is prepared by ball milling and mixing graphite tailings, quartz, bauxite, feldspar and silicon carbide in sequence, adding water for granulation, preparing blanks, ageing, pressing, firing and the like. The invention needs to add high-quality mineral substances such as quartz, bauxite, feldspar and the like while utilizing the graphite tailings, thereby improving the preparation cost of the foamed ceramic. Similarly, the method also comprises a Chinese invention patent CN11205103A, 40-70% of graphite tailings and kaolin and feldspar for preparing the light ceramic tile. Obviously, in the above prior art schemes, the graphite tailings are used together with the concentrate to prepare the hollow brick or the perforated brick, and when the addition amount of the graphite tailings is too large, the mechanical properties of the product can be seriously affected, and meanwhile, especially when the partition board is prepared by adopting the above prior art, the mechanical properties cannot meet the requirements.
In summary, in the prior art, the comprehensive utilization of the graphite picking and selecting solid wastes has the following problems: (1) the method still stays in the research of single graphite ore dressing tailings, has less research on the combined utilization of the stripped clay, the mining waste rock and the like, and particularly considers that the combined utilization of the mining waste rock and other solid wastes cannot obtain the foamed ceramic material meeting the requirements; (2) the addition amount of the graphite tailings is generally not more than 70%, and a certain amount of external high-quality resources such as kaolin, quartz, feldspar and the like still need to be added, so that the dependence degree on the high-quality resources is high; (3) the mechanical property of the ceramic material is easily reduced when the addition amount of the graphite solid waste is too high, particularly when the addition amount of mining waste stone is too high, and the mechanical property of the partition board building material cannot meet the requirement particularly when the partition board building material is prepared.
Disclosure of Invention
The invention aims to provide a graphite-based multi-source solid waste foamed ceramic material, a preparation method thereof and a partition board, wherein graphite tailings are used as a main raw material, graphite ore dressing tailings are used as a main material, clay stripping and mining waste rocks are used as auxiliary materials, the solid waste of graphite mining and dressing is systematically utilized, no high-quality ore source is required to be added, the dependence degree on external high-quality resources is greatly reduced, and particularly the mining waste rocks are fully utilized, so that the high-quality resources are saved, and the cost is reduced; meanwhile, the prepared foamed ceramic partition board has good mechanical property and heat-conducting property.
In order to achieve the purpose, the invention provides a graphite-based multi-source solid waste-based foamed ceramic material which comprises, by mass, 50-70% of graphite ore dressing tailings, 5-20% of mining waste rocks, 5-25% of exfoliated clay and 0-15% of auxiliary binder. Wherein, the main component of the graphite ore dressing tailings is SiO in percentage by mass2The content is more than or equal to 50 percent, and the content of other components is Al2O3 5～15％、Fe2O3 0～10％、 CaO+MgO 0～20％、K2O+Na20-5% of O and 1-3% of residual graphite; the mining waste rock mainly comprises SiO2And CaO, SiO230-50% of CaO, 15-30% of CaO and Al as the other component2O3 5～15％、Fe2O3 0～10％、MgO 0～5％、K2O+Na20-5% of O; main composition of exfoliated clayIs divided into SiO2And Al2O3，SiO230-50% of Al2O315-30% of the total weight of the composition, and Fe as the other component2O3 0～10％、CaO+MgO 0～5％、K2O+Na2O 0～5％。
Further, the auxiliary binder is kaolin and/or feldspar.
Further, the foaming agent is 0-0.5%. Still further, the foaming agent is silicon carbide.
Further, the sum of the addition amounts of the graphite ore dressing tailings and the mining waste rock is as follows by mass ratio: stripping clay: adhesive: 70-90% of foaming agent: 5-25%: 5-10%: 0.2-0.5%; preferably, the sum of the addition amounts of the graphite mill tailings and the mining waste rock is as follows: stripping clay: kaolin: 70-85% of silicon carbide: 10-15: 10: 0.5; most preferably, the sum of the addition amounts of the graphite mill tailings and the mining waste rocks is: stripping clay: adhesive: foaming agent 80: 10: 10: 0.5.
further, the foamed ceramic material is prepared by mixing graphite ore dressing tailings, mining waste stones, exfoliated clay, an auxiliary binder and/or a foaming agent and then carrying out a pugging process.
On the other hand, in order to achieve another purpose of the invention, the invention provides a preparation method of a graphite-based multi-source solid waste foamed ceramic material, which comprises the following steps:
(1) mixing materials: uniformly mixing graphite ore dressing tailings, mining waste rocks, stripped clay, an auxiliary binder and a foaming agent in proportion to prepare a mixed material;
(2) preparing slurry: adding water into the mixed material, and performing wet ball milling to obtain slurry;
(3) and (3) dehydrating: dehydrating the slurry prepared in the step (2) to prepare a wet material;
(4) pugging: pugging the wet material to obtain;
(5) and (3) ageing and drying: sealing and ageing the pugging material for 24-48 h, and drying the aged wet material; the function of staleness mainly comprises that the moisture is distributed more evenly, and at the same time, under the action of bacteria, the organic substances contained in the materials are fermented, oxidation-reduction reaction is carried out, the generated gas is diffused and flows, so that the wet materials are more evenly promoted, and the plasticity of the mixed materials is improved.
The dried material is scattered to form powder. And distributing the powder in a mold, pressing into a blank according to the requirement and then firing.
Further, the ball milling fineness of the step (2) is 100 meshes to +300 meshes, and the passing rate is 100%; after ball milling, 100 percent of the mixed material is sieved by a 100-mesh sieve, so that iron in the mineral aggregate is sieved and can be recycled.
Further, the moisture content of the wet material in the step (3) is 30-60%.
Further, the frequency of the pugging process in the step (4) is 3-5 times.
Further, the moisture content after drying in the step (5) is less than or equal to 3 percent.
The partition board obtained by sintering the foamed ceramic material or the foamed ceramic material prepared by the method comprises the step of sintering a material or a blank prepared from the foamed ceramic material in a high-temperature furnace, wherein the sintering temperature is 1100-1200 ℃, and the heat preservation time is 30-90 min.
Similarly, the foamed ceramic material prepared by the present invention can be used as a firing raw material for preparing other building materials.
The invention principle of the invention is as follows:
the invention selects three major solid wastes of graphite as main raw materials, which respectively comprise exfoliated clay, mining waste stone and mineral dressing tailings, wherein the addition amount of the three major solid wastes in the preparation of the foamed ceramic material can be more than 90 percent, so that the consumption of the solid wastes in high efficiency and batch is realized, and the prepared foamed ceramic material and the partition board can meet the standard requirements.
Firstly, analyzing the main components of each solid waste, wherein the main component of the mineral processing tailings is silicon dioxide, and the main components of the mining waste rocks are calcium oxide and silicon dioxide; the main component of the exfoliated clay is an aluminum clay containing a relatively high content of alumina, or the like. According to the main components of the three solid wastes, the mining waste rocks are similar to the main components of quartz and feldspar minerals in high-quality minerals, and the exfoliated clay can completely or partially replace high-quality kaolin. Comprehensively, the main components of the exfoliated clay, the mining waste rock and the mineral processing tailings comprise silicon dioxide, calcium oxide and aluminum oxide. After the three mineral raw materials are mixed, the foamed ceramic partition wall board wall material is prepared by exerting the synergistic advantages of the components of different types of solid wastes, so that the dependence on external high-quality resources can be greatly reduced, and the addition amount of the solid wastes is increased.
On one hand, silica, calcium oxide, alumina and the like are converted into anorthite, mullite and other crystal phases at high temperature, the anorthite and the mullite have the characteristics of high hardness, high stability, good mechanical properties and the like, and the mechanical strength of the foamed ceramic can be obviously improved; meanwhile, components such as silicon dioxide and the like can form a glass state (liquid phase state) under a high temperature condition, and are filled among crystals to be tightly combined, so that the mechanical strength of the foamed ceramic is improved.
On the other hand, in order to fully exert the plasticity of poor-quality aluminum raw materials such as exfoliated clay and the like and improve the addition amount of the exfoliated clay and the mechanical strength of the foamed ceramic material, the invention dehydrates slurry to obtain wet material, performs a pugging process when the water content is controlled to be 30-60%, performs rolling pugging on the wet material for 3-5 times to obtain a highly mixed material, and improves the plasticity and the adhesive property of the material. According to the invention, through the composite proportioning of the mineral tailings, the mining waste rocks and the exfoliated clay and the treatment of the pugging process, the full utilization of the mineral tailings and the mining waste rocks is realized, the adverse effect on the foamed ceramic material caused by the overhigh content of the exfoliated clay is effectively solved, and the remarkable improvement of the addition amount of the graphite solid waste in the foamed ceramic is realized. Meanwhile, the water content of the pugging process plays an important role, so that the mixing uniformity of the blank is improved through pugging, and the plasticity and the bonding property of the blank can be improved. However, when the moisture content is less than 20%, a dry and hard mud state occurs in the pugging process, so that the subsequent blank has uneven density, and the heat-conducting property and the compression resistance of the partition board are poor. When moisture reaches 70%, cause the high energy consumption of dehydration technology on the one hand, on the other hand coefficient of heat conductivity is not high, and the analysis reason probably leads to the viscosity high with the humidity is too high in the foaming process, and the inside unable even bubble that obtains of wet material leads to the foaming rate not high, influences the void fraction in the partition plate to make the adoption density too big, improved the cost of unit volume on the one hand, on the other hand influences the utilization cost in the use of the product of foamed ceramic material preparation.
Meanwhile, the graphite remained in the mineral dressing tailings is uniformly distributed in each crystal and can be oxidized to generate gas under the high-temperature condition, uniform air holes are formed in the ceramic, the porosity of the foamed ceramic is improved, and the heat insulation performance of the foamed ceramic is improved; meanwhile, the oxidation of the residual graphite can reduce the sintering temperature of the ceramic and improve the uniformity of liquid phase distribution, thereby improving the compressive strength of the sintered foamed ceramic material.
Specifically, the formation of the glass state is characterized in that a multi-element eutectic calcium oxide-alumina-silica is formed during high-temperature sintering, so that the sintering temperature is reduced, the melting in a system is promoted, the calcium oxide-alumina-silica is diffused and permeated in a liquid phase to accelerate the formation of mullite, and anorthite glass bodies generated in the melting process are filled among mullite grains, so that a blank is compact, gaps are reduced, a framework structure is formed, and the mechanical strength of a ceramic blank is improved; meanwhile, graphite flake particles are uniformly distributed in the anorthite structure and oxidized to generate gas at high temperature, so that the foaming and pore-forming effects are achieved, pores of the foamed ceramic product are uniformly distributed, the thermal expansion coefficient is reduced, and the thermal insulation performance of the foamed ceramic is improved. Because of the generation of crystal phases such as anorthite, mullite and the like, the strength of the foamed ceramic is improved, and the mechanical property of the foamed ceramic product is promoted. Meanwhile, feldspar and/or kaolin are selected as a binder, the main components of the feldspar and/or kaolin are alumina and silicon dioxide, and presumably, the binder acts with calcium oxide in high-temperature sintering to promote the formation of eutectic, and is equivalent to a foaming promoter, so that the binder forms low eutectic with the calcium oxide to form a crystal nucleus forming process, thereby promoting the formation of mullite, reducing the sintering temperature and promoting the foaming and pore-forming speed. Through the analysis of the above principle, through optimizing the proportion of three kinds of solid wastes, when the graphite ore dressing tailings and the sum of the addition of mining barren rocks: 70-85% of exfoliated clay: 10-15 can obtain high compressive strength under the condition of low density, obviously, the three have synergistic effect, and the compactness and the porosity of the foamed ceramic material are improved, so that the foamed ceramic material has the characteristics of low density and high strength (mechanical property). Through the application of the technical scheme, compared with the prior art, the invention has the following advantages:
1. by adopting the technical scheme of the invention, the defect of low addition amount of mining waste rock in the prior art is overcome, better mechanical property can be obtained when the addition amount is more than 10%, a partition plate product meeting the national standard is prepared, the traditional cognition that the mechanical property of a ceramic material is reduced due to the addition of a large amount of mining waste rock, so that the mechanical property of the material cannot meet the requirement is abandoned, and the mining waste rock for a long time cannot be effectively utilized in the product with higher requirement on the mechanical property; the addition amount of the mining waste rock reaches 20%, and the partition board material with high compressive strength can be obtained by performing synergistic effect in cooperation with the comprehensive application of other solid wastes, so that the new application of the mining waste rock is developed, and the use way of graphite mining and selecting solid wastes in building materials is widened.
2. By adopting the technical scheme of the invention, the graphite mining and selecting solid waste such as the exfoliated clay, the mining waste rock, the mineral processing tailings and the like is systematically utilized, three poor-quality resources of the graphite tailings are comprehensively utilized according to the proportioning design, no high-quality mineral resources are required to be added, the degree of dependence on external high-quality clay resources such as kaolin, feldspar and the like is greatly saved, the problem of mechanical property reduction of foamed ceramics caused by excessively high addition of the poor-quality mineral resources in the prior art is solved, the comprehensive utilization of the graphite multi-source solid waste is realized, the production cost is reduced, meanwhile, the consumption conveying of batch poor-quality solid waste to the building industry is realized, and the virtuous cycle of graphite mineral mining is promoted.
3. By adopting the technical scheme of the invention, graphite mining solid wastes such as stripped clay, mining waste rock, mineral dressing tailings and the like are systematically utilized, and the comprehensive utilization rate of the solid wastes is high and can reach 90% under the condition of meeting the requirements of the current standard; the dependence degree on external high-quality clay resources such as kaolin, feldspar and the like is greatly saved, the self comprehensive utilization of graphite multi-source solid waste is realized, the production cost is reduced, meanwhile, the consumption conveying of batch inferior solid waste to the building industry is realized, the land occupation amount is reduced, the pollution to air, water sources and land is relieved, and the virtuous cycle of graphite mineral exploitation is promoted.
4. By adopting the technical scheme of the invention, the foamed ceramic material with excellent mechanical property, thermal insulation property, breaking strength and fireproof property is obtained, the existing processing equipment can be directly utilized, the operation is simple, only a small amount of binder and foaming agent needs to be added, the production, material and equipment costs are saved, and the method is suitable for large-scale popularization and production.
5. According to the invention, the pugging process is added in the preparation process of the foamed ceramic, so that the plasticity and the cohesiveness of the inferior solid waste resource are fully improved, the effectiveness of the inferior solid waste resource as a binding material is improved, and the comprehensive performances of compression resistance, heat conduction, sound insulation and the like of the foamed ceramic material can be improved while the addition amount of the solid waste is increased. Meanwhile, the high mixing of materials can be improved, and a firing basis is provided for improving the compactness and the uniformity of pores of the foamed ceramic blank in a firing process, so that the mechanical property, the mechanical property and the heat insulation property of the foamed ceramic material are improved.
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described below with reference to the specific contents of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments of the present invention without making any creative effort, shall fall within the protection scope of the present invention.
The invention discloses a graphite-based multi-source solid waste foamed ceramic material, which comprises the following steps:
(1) mixing materials: the graphite ore dressing tailings, the mining waste rocks, the exfoliated clay, the auxiliary binder and the foaming agent are uniformly mixed according to a proportion to prepare a mixed material. Wherein the auxiliary binder is kaolin and/or feldspar, and the foaming agent is silicon carbide. The above raw materials are crushed in advance and then mixed. Wherein, the silicon carbide is sieved by a 700-mesh sieve, and other raw materials are sieved by a 230-mesh sieve.
(2) Slurry preparation: and adding water into the mixed material, carrying out wet ball milling to obtain slurry, and adding the mixed material after adding the water into a ball mill at the rotating speed of 20-30 r/min. After ball milling, screening by a vibrating screen, and removing iron, wherein the fineness is 100-300 meshes, and the passing rate is 100%.
(3) And (3) dehydrating: and (3) dehydrating the slurry prepared in the step (2) to prepare a wet material.
(4) Pugging: pugging the wet material to obtain; and adding the wet material into the stirred mud, and performing vacuum pugging for 2-3 times. Specifically, the pugging process comprises the following steps: and (3) putting the wet material into a mud stirring machine, stirring and cutting the wet material through a helical blade, carrying out vacuum treatment under the vacuum degree of 0.1MPa, wherein the mud discharging speed is 1m/min, extruding mud segments, and repeating for 2-3 times. When the pugging process is used, bubbles in the wet material are removed through stirring and extrusion, so that the wet material is highly and uniformly mixed, the moisture content is uniform, and the plasticity of the mixed material is improved.
(5) And (3) ageing and drying: sealing and ageing the pugging material for 24-48 h, drying the aged wet material, and firing the dried material to obtain the required foamed ceramic product.
The technical solution of the present invention is further illustrated by the following specific examples.
In the following examples, the main component of the selected graphite mill tailings is SiO in percentage by mass2The content is more than or equal to 50 percent; the other component content is Al2O3 5～15％、Fe2O3 0～10％、CaO+MgO 0～20％、 K2O+Na20-5% of O and 1-3% of residual graphite.
The mining waste rock comprises the main component of SiO in percentage by mass2And CaO, SiO2The content is 30-50%, and the content of CaO is 15-30%; the other component content is Al2O3 5～15％、Fe2O3 0～10％、 MgO 0～5％、K2O+Na2O 0～5％。
The main component of the exfoliated clay is SiO in percentage by mass2And Al2O3，SiO2The content is 30-50％，Al2O3The content is 15-30%; the other component content is Fe2O3 0～10％、CaO+MgO 0～5％、 K2O+Na2O 0～5％。
The pugging process adopts a 250-type ceramic vacuum pugging machine, Xinlong mechanical factory in Heshan area, Hubei city.
Example 1
The embodiment comprises the following steps:
(1) 69.5 percent of graphite ore dressing tailings, 20 percent of mining waste stone, 5 percent of stripping clay, 5 percent of kaolin and 0.5 percent of silicon carbide are uniformly mixed according to the mass percentage to prepare a mixed material.
(2) And adding water into the mixed material, and performing wet ball milling to obtain slurry.
(3) And (3) dehydrating the slurry prepared in the step (2) to prepare a wet material, wherein the water content of the wet material is 30%.
(4) And (4) carrying out pugging process treatment on the wet material obtained in the step (3), wherein the pugging time is 3 times.
(5) Sealing and ageing the pugging material obtained in the step (4) for 24-48 h, and drying the aged material, wherein the moisture content after drying is less than or equal to 3%.
And (3) scattering the dried materials to form powder, and injecting the powder into a grinding tool to press the powder to form a blank.
Example 2
The difference between the present example and example 1 is that the raw materials are different in mixture ratio, and in the present example, the mixture ratio is 69.5% of graphite mill tailings, 10% of mining waste rock, 15% of exfoliated clay, 5% of kaolin and 0.5% of silicon carbide, which are calculated by mass percentage.
Example 3
The difference between the present example and example 1 is that the raw materials are different in mixture ratio, and in the present example, the mixture ratio is 69.5% of graphite mill tailings, 5% of mining waste rock, 20% of exfoliated clay, 5% of kaolin and 0.5% of silicon carbide, which are calculated by mass percentage.
Example 4
The difference between the present example and example 1 is that the raw materials are different in mixture ratio, and in the present example, the mixture ratio is 69.5% of graphite mill tailings, 10% of mining waste rock, 10% of exfoliated clay, 10% of kaolin, and 0.5% of silicon carbide, which are calculated by mass percentage.
Example 5
The difference between the embodiment and the embodiment 1 is that the raw material mixture ratio is different, in the embodiment, the mixture ratio is 49.5% of graphite mill tailings, 20% of mining waste rock, 20% of exfoliated clay, 10% of kaolin and 0.5% of silicon carbide, which are calculated by mass percentage.
Example 6
The difference between the present example and example 1 is that the raw materials are different in mixture ratio, and in the present example, the mixture ratio is 49.8% of graphite mill tailings, 20% of mining waste rock, 20% of exfoliated clay, 10% of kaolin and 0.2% of silicon carbide, which are calculated by mass percentage.
Example 7
The difference between the embodiment and the embodiment 1 is that the raw materials are different in proportion, in the embodiment, the proportion of the mixed materials is 69.5% of graphite mill tailings, 20% of mining waste rock, 5% of exfoliated clay, 5% of feldspar and 0.5% of silicon carbide, and the above are calculated by mass percentage.
Example 8
The difference between the embodiment and the embodiment 1 is that the raw materials are different in proportion, in the embodiment, the proportion of the mixed materials is 69.5% of graphite mill tailings, 20% of mining waste rock, 5% of exfoliated clay, 2.5% of feldspar, 2.5% of kaolin and 0.5% of silicon carbide, and the above are calculated by mass percentage.
Example 9
The difference between the present example and example 1 is that the raw materials are different in mixture ratio, and in the present example, the mixture ratio is 49.5% of graphite mill tailings, 20% of mining waste rock, 25% of exfoliated clay, 5% of kaolin and 0.5% of silicon carbide, which are calculated by mass percentage.
Example 10
The difference between the present example and example 1 is that the raw materials are different in mixture ratio, and in the present example, the mixture ratio is 49.5% of graphite mill tailings, 20% of mining waste rock, 15% of exfoliated clay, 15% of kaolin, and 0.5% of silicon carbide, which are calculated by mass percentage.
Example 11
The difference between the present example and example 1 is that the raw materials are different in mixture ratio, and in the present example, the mixture ratio is 74.5% of graphite mill tailings, 10% of mining waste rock, 10% of exfoliated clay, 5% of kaolin, and 0.5% of silicon carbide, which are calculated by mass percentage.
Example 12
The difference between the present example and example 1 is that the raw materials are different in mixture ratio, and in the present example, the mixture ratio is 59.5% of graphite mill tailings, 15% of mining waste rock, 15% of exfoliated clay, 10% of kaolin and 0.5% of silicon carbide, which are calculated by mass percentage.
Example 13
The difference between the present example and example 1 is that the raw materials are different in mixture ratio, and in the present example, the mixture ratio is 64.5% of graphite mill tailings, 15% of mining waste rock, 10% of exfoliated clay, 10% of kaolin, and 0.5% of silicon carbide, which are calculated by mass percentage.
Example 14
The difference between the present example and example 1 is that the raw materials are different in mixture ratio, and in the present example, the mixture ratio is 59.5% of graphite mill tailings, 20% of mining waste rock, 10% of exfoliated clay, 10% of kaolin, and 0.5% of silicon carbide, which are calculated by mass percentage.
Example 15
The difference between the embodiment and the embodiment 1 is that the mixture ratio of the raw materials is different, in the embodiment, the ratio of the mixed materials is 54.5% of the graphite mill tailings, 25% of the mining waste rock, 10% of the exfoliated clay, 10% of the kaolin and 0.5% of the silicon carbide, which are calculated by mass percentage.
Example 16
This example is different from example 1 in that the moisture of the wet mass produced in the dehydration process of step (3) is 40%.
Example 17
This example is different from example 1 in that the moisture of the wet material produced in the dehydration process of step (3) is 60%.
Example 18
The difference between the present embodiment and embodiment 1 is that silicon carbide is not added as a foaming agent, and the mixture ratio of the raw materials is different, in the present embodiment, the ratio of the mixed materials is 70% of mineral tailings, 15% of mining waste rock, 15% of exfoliated clay, and 5% of kaolin, which are all calculated by mass percentage.
Example 19
The difference between the present example and example 1 is that no silicon carbide is added as a foaming agent, and the mixture ratio of the raw materials is different, in the present example, the proportions of the mixed materials are 60% of the mineral tailings, 20% of the mining waste rock, 15% of the exfoliated clay, and 5% of the kaolin, which are calculated by mass percentage.
Example 20
This example differs from example 1 in that the number of puggings was 5.
Comparative example 1
The comparative example includes the following steps:
(1) 74.5 percent of graphite ore dressing tailings, 15 percent of mining waste stone, 10 percent of stripping clay and 0.5 percent of silicon carbide are uniformly mixed according to the weight percentage to prepare a mixed material.
(2) And adding water into the mixed material, and performing wet ball milling to obtain slurry.
(3) And (3) dehydrating the slurry prepared in the step (2) to prepare a wet material, wherein the water content of the wet material is 30%.
(4) And (4) carrying out pugging process treatment on the wet material obtained in the step (3), wherein the pugging time is 3 times.
(5) Sealing and ageing the pugging material obtained in the step (4) for 24-48 h, and drying the aged material, wherein the moisture content after drying is less than or equal to 3%.
(6) And (5) scattering the dried material and pressing the material into a blank.
Comparative example 2
The comparative example includes the following steps:
(1) 69.5 percent of graphite ore dressing tailings, 5 percent of quartz, 10 percent of bauxite, 15 percent of feldspar and 0.5 percent of silicon carbide are uniformly mixed according to the proportion to prepare a mixed material, and the components are calculated according to the mass percentage.
(2) And adding water into the mixed material, and performing wet ball milling to obtain slurry.
(3) And (3) dehydrating the slurry prepared in the step (2) to prepare a wet material, wherein the water content of the wet material is 30%.
(4) And (4) carrying out pugging process treatment on the wet material obtained in the step (3), wherein the pugging time is 3 times.
(5) Sealing and ageing the pugging material obtained in the step (4) for 24-48 h, and drying the aged material, wherein the moisture content after drying is less than or equal to 3%.
(6) And (5) scattering the dried material and pressing the material into a blank.
Comparative example 3
(1) 69.5 percent of graphite ore dressing tailings, 20 percent of kaolin, 10 percent of feldspar and 0.5 percent of silicon carbide are uniformly mixed according to the proportion to prepare a mixed material, and the components are calculated according to the mass percentage.
(2) And adding water into the mixed material, and performing wet ball milling to obtain slurry.
(3) And (3) dehydrating the slurry prepared in the step (2) to prepare a wet material, wherein the water content of the wet material is 30-60%.
(4) And (4) carrying out pugging process treatment on the wet material obtained in the step (3), wherein the pugging time is 3 times.
(5) Sealing and ageing the pugging material obtained in the step (4) for 24-48 h, and drying the aged material, wherein the moisture content after drying is less than or equal to 3%.
(6) And (5) scattering the dried material and pressing the material into a blank.
Comparative example 4
(1) 69.5 percent of graphite ore dressing tailings, 20 percent of kaolin, 10 percent of feldspar and 0.5 percent of silicon carbide are uniformly mixed according to the proportion to prepare a mixed material, and the components are calculated according to the mass percentage.
(2) And adding water into the mixed material, and performing wet ball milling to obtain slurry.
(3) Grinding the particles obtained by ball milling to be less than or equal to 74 mu m, then drying, and crushing to be less than or equal to 150 mu m after drying to be used as powder.
(4) And (5) scattering the dried material and pressing the material into a blank.
Comparative example 5
The comparative example is different from example 1 in that the moisture of the wet material obtained in the dehydration process of step (3) is 20%.
Comparative example 6
The comparative example is different from example 1 in that the moisture of the wet material obtained in the dehydration process of step (3) is 70%.
Comparative example 7
The difference between the comparative example and the example 1 lies in the different proportions of the raw materials, in the present example, the proportions of the mixed materials are 49.5% of graphite mill tailings, 30% of mining waste rock, 10% of exfoliated clay, 10% of kaolin and 0.5% of silicon carbide, which are calculated by mass percentage.
Comparative example 8
The difference between the comparative example and the example 1 is that the raw materials are different in proportion, and the proportion of the mixed materials is 49.5% of graphite ore dressing tailings, 10% of mining waste rock, 30% of stripping clay, 10% of kaolin and 0.5% of silicon carbide, which are calculated by mass percentage.
Comparative example 9
The difference between the comparative example and the example 1 is that silicon carbide is not added as a foaming agent, the mixture ratio of the raw materials is different, and in the comparative example, the proportion of the mixed materials is 45% of graphite ore dressing tailings, 15% of mining waste rock, 20% of exfoliated clay and 20% of kaolin, which are calculated by mass percentage.
Comparative example 10
The difference between this comparative example and example 1 is that no silicon carbide is added as a foaming agent, and the raw materials are in different proportions, in this example, the proportions of the mixed materials are 40% of graphite mill tailings, 20% of mining waste rock, 20% of exfoliated clay, and 20% of kaolin, all of which are calculated by mass percentage.
Comparative example 11
The comparative example is different from example 1 in that the number of pugging operations is 7, and the rest is the same as example 1.
Comparative example 12
The difference between the comparative example and the example 1 is that the dewatered wet material is directly aged and sealed without pugging process, and other steps are the same as the example 1.
And (3) distributing the powder or the blank obtained in the embodiment and the comparative example in a mold, then sintering in a high-temperature furnace, cooling, demolding and cutting to obtain the partition board, wherein the sintering temperature is 1100-1200 ℃, and the heat preservation time is 30-90 min.
The partition plate obtained by cutting has the size of 1500mm in length, 500mm in width and 90mm in thickness.
The prepared partition board is detected according to the building industry standard T/CBCSA12-2019 foaming ceramic partition board, and the volume density is detected according to the method specified in the standard.
Other performance detection methods are respectively as follows:
the compressive strength was measured according to the regulations of GB/T23451-2009 light partition wall panels for construction.
The thermal conductivity is measured according to GB/T10294-.
The combustion performance was measured according to the regulations of GB8624-1997 method for grading the combustion performance of building materials.
The results are shown in Table 1.
Wherein the average temperature of the heat conductivity coefficient is 25 +/-2 ℃; the bending-resistant load refers to the plate dead weight multiple.
According to the physical property parameters in table 1, the partition boards prepared in examples 1 to 20 can meet the requirements of T/CBCSA12-2019 "foamed ceramic partition board" on heat insulation and preservation materials, that is, the indexes are evaluated by the product index with the density index of 500: water absorption rate less than or equal to 1.5% and combustion performance A1The density is not less than 480 and not more than 540, the average compressive strength is not less than 7.0MPa (hereinafter referred to as compressive strength), and the thermal conductivity is not more than 0.35W/(m.K).
Examples 1-20, the sum of the addition of graphite mill tailings and mining waste rock are given: clay exfoliation: kaolin: 70-90% of silicon carbide: 5-25: 5-10: the formula proportion of 0.2-0.5, and the detection result shows that the foamed ceramic material prepared by the technical scheme of the invention has better mechanical property (compressive strength), and the heat conductivity (heat conductivity coefficient) and combustion performance of the foamed ceramic material meet the requirements.
Specifically, as can be seen from examples 1 to 6 and examples 9 to 15, the other conditions are the same, and by changing the addition ratio of the graphite mill tailings and the mining waste rock, when the sum of the addition amounts of the graphite mill tailings and the mining waste rock is: the mass ratio of the exfoliated clay is 80: 10 is the best, and the sum of the addition amounts of the graphite ore dressing tailings and the mining waste rocks is as follows: the mass ratio of the exfoliated clay is 75-85: 10 to 15 times.
Meanwhile, in combination with comparative examples 7-8, when 30% of mining waste rock is found in comparative example 7, the mechanical property of the partition board is rapidly reduced, and the requirements of the standard on the mechanical property of the partition board are obviously not met. Meanwhile, in the comparative examples 7-8, under the same conditions of graphite ore dressing tailings, the mining waste rock is reduced, the content of the exfoliated clay is increased, and the results show that the water absorption rate and the compressive strength do not reach the standard.
As can be seen from examples 1 and 7-9, feldspar or kaolin was chosen as the binder with comparable results.
Examples 1, 16-17 and comparative examples 5-6 the comparative experiments on the moisture content of the wet material obtained in the dehydration process of step (3) showed that the partition boards obtained by the method were not satisfactory as compared with the examples. In comparative example 5, dry and hard mud appeared in the pugging process, while in comparative example 6, the viscosity was found to be too high in the pugging process, and the processing was difficult.
In comparison with comparative examples 8-9, examples 18-19 did not contain any blowing agent, and the partition boards prepared in comparative examples 8-9 were unsatisfactory. Compared with the partition boards prepared in the examples 18 to 19, the partition boards are different in foaming performance and can meet the standard requirements. Specifically, it was analyzed that, in comparative example 8, when 30% of the exfoliated clay was added, the water absorption and thermal conductivity were significantly unable to meet the standard requirements. In contrast, in comparative example 9, when the amount of the graphite mill tailings is as low as 45% without adding the foaming agent, the foaming performance is obviously poor, and it is obvious that the graphite mill tailings have a promoting effect on the sintering principle of the foamed ceramic material. The graphite ore dressing tailings contain partial residual flake graphite, and graphite flake particles are uniformly distributed in the structure of anorthite and oxidized to generate gas under the high-temperature condition, so that the foaming and pore-forming effects are achieved, pores of a foamed ceramic product are uniformly distributed, the thermal expansion coefficient is reduced, and the heat insulation performance of the foamed ceramic is improved. Therefore, when the addition of the graphite mill tailings is too low and no foaming agent exists, the gas generated by the residual graphite in the sintering process is insufficient, and bubbles meeting the requirement are generated to form gaps.
The increase of the number of times of the pugging process contributes to the improvement of the performance of the partition wall board by comparing example 1, example 20, comparative example 11 and comparative example 12, but it can be seen that the performance of the partition wall board cannot be improved by 7 times of the pugging process by example 20 and comparative example 11, and 3 to 5 times of the pugging process is preferable in terms of the process cost. Comparative example 12 did not pass through the pugging process, and the mechanical properties were significantly reduced, because the pugging process could improve the plasticity of the exfoliated clay, and could make the pug more compact and uniform, and the sintered foamed ceramic material had high compactness and improved compressive strength.
As can be seen from comparative examples 3 and 4, the mechanical properties of the partition board prepared by the technical scheme of the prior art are not satisfactory. However, it can also be seen that the performance of the partition board prepared by the preparation method of the invention in the comparative example 3 is superior to that of the partition board prepared by other preparation methods in the prior art.
Obviously, the graphite tailings are adopted as main raw materials, the graphite tailings comprise graphite ore dressing tailings, mining waste rocks and stripping clay, the total addition amount of the graphite ore dressing tailings, the mining waste rocks and the stripping clay can reach 95%, the reasonable proportion of the graphite ore dressing tailings, the mining waste rocks and the stripping clay can be fully utilized, the mutual synergistic effect of main components of the graphite ore dressing tailings, the mining waste rocks and the stripping clay can be realized, the excellent mechanical property can be realized, and obviously, the mechanical property meets the requirement of the national standard of the partition board. According to the embodiment, when the sum of the addition amounts of the graphite ore dressing tailings and the mining waste rock is as follows: stripping clay: kaolin: 70-90% of silicon carbide: 5-25: 5-10: the performance of the partition board prepared by the foamed ceramic material prepared at 0.2-0.5 time meets the standard requirement; further, when the sum of the addition amounts of the graphite ore dressing tailings and the mining waste rocks is as follows: clay exfoliation: kaolin: 70-85% of silicon carbide: 10-15: 10: 0.5 times; as the best mode, the sum of the addition amount of the graphite ore dressing tailings and the mining waste rock, the addition amount of the exfoliated clay, the kaolin and the silicon carbide is 80: 10: 0.5, and the best mode is.
Table 1 physical property parameter table of foamed ceramic partition board
Figure BDA0003564158880000161
The method takes graphite multi-source solid waste as a main raw material, reduces the raw material cost of the product, provides a new and effective way for recycling solid waste resources, and has positive significance for efficiently reducing the accumulation pressure of the solid waste and reducing environmental pollution and land occupation resources.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.

Claims (10)

1. The foamed ceramic material based on graphite multi-source solid waste is characterized by comprising, by mass, 50-70% of graphite ore dressing tailings, 5-20% of mining waste rocks, 5-25% of exfoliated clay and 0-15% of auxiliary binders.
2. The graphite-based multi-source solid waste foamed ceramic material of claim 1, wherein the auxiliary binder is kaolin and/or feldspar.
3. The graphite-based multi-source solid waste foamed ceramic material of claim 1 or 2, further comprising 0-0.5% by mass of a foaming agent; the foaming agent is silicon carbide.
4. The foamed ceramic material based on graphite multi-source solid waste of claim 3, wherein the sum of the addition amounts of graphite mill tailings and mining waste rocks is calculated according to the mass ratio: stripping clay: auxiliary binder: 70-90% of foaming agent: 5-25: 5-10: 0.2 to 0.5.
5. The foamed ceramic material based on graphite multisource solid waste of claim 4, characterized in that the foamed ceramic material is prepared by mixing graphite mill tailings, mining waste rock, exfoliated clay, auxiliary binder and/or foaming agent and subjecting the mixture to pugging process.
6. The preparation method of the graphite-based multi-source solid waste-based foamed ceramic material according to any one of claims 1 to 5, comprising the following steps:
(1) mixing materials: uniformly mixing graphite ore dressing tailings, mining waste rocks, stripped clay, an auxiliary binder and a foaming agent in proportion to prepare a mixed material;
(2) preparing slurry: adding water into the mixed material, and performing wet ball milling to obtain slurry;
(3) and (3) dehydrating: dehydrating the slurry prepared in the step (2) to prepare a wet material;
(4) pugging: carrying out pugging process treatment on the wet material;
(5) and (3) ageing and drying: sealing and ageing the pugging material for 24-48 h, and drying the aged wet material;
(6) preparing a blank: and scattering the dried material to obtain powder, and pressing into a blank of the foamed ceramic material.
7. The preparation method of the foamed ceramic material based on graphite multi-source solid waste of claim 6, wherein the ball milling fineness of the step (2) is 100 to +300 meshes of pass rate.
8. The preparation method of the foamed ceramic material based on graphite multi-source solid waste of claim 6, wherein the moisture content of the wet material in the step (3) is 30-60%.
9. The preparation method of the foamed ceramic material based on graphite multi-source solid waste of claim 6, wherein the number of pugging processes in the step (4) is 3-5.
10. The partition board is prepared from the foamed ceramic material according to any one of claims 1 to 5 or the foamed ceramic material prepared by the preparation method according to any one of claims 6 to 9, and comprises the step of firing a blank prepared from the foamed ceramic material in a high-temperature furnace, wherein the firing temperature is 1100-1200 ℃, and the heat preservation time is 30-90 min.
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