CN111747725A - Foamed ceramic material, decorative plate and preparation method - Google Patents

Foamed ceramic material, decorative plate and preparation method Download PDF

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Publication number
CN111747725A
CN111747725A CN202010687847.7A CN202010687847A CN111747725A CN 111747725 A CN111747725 A CN 111747725A CN 202010687847 A CN202010687847 A CN 202010687847A CN 111747725 A CN111747725 A CN 111747725A
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China
Prior art keywords
parts
foaming
foamed ceramic
ceramic material
coal gangue
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Inventor
娄广辉
王治
徐开东
尹蕊
金彪
张国富
李峰
尹星
张璐
李璐洋
王安
常永
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Henan Building Material Research And Design Institute Co ltd
Henan University of Urban Construction
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Henan Building Material Research And Design Institute Co ltd
Henan University of Urban Construction
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Priority to CN202010687847.7A priority Critical patent/CN111747725A/en
Publication of CN111747725A publication Critical patent/CN111747725A/en
Pending legal-status Critical Current

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    • EFIXED CONSTRUCTIONS
    • E04BUILDING
    • E04FFINISHING WORK ON BUILDINGS, e.g. STAIRS, FLOORS
    • E04F13/00Coverings or linings, e.g. for walls or ceilings
    • E04F13/07Coverings or linings, e.g. for walls or ceilings composed of covering or lining elements; Sub-structures therefor; Fastening means therefor
    • E04F13/08Coverings or linings, e.g. for walls or ceilings composed of covering or lining elements; Sub-structures therefor; Fastening means therefor composed of a plurality of similar covering or lining elements
    • E04F13/14Coverings or linings, e.g. for walls or ceilings composed of covering or lining elements; Sub-structures therefor; Fastening means therefor composed of a plurality of similar covering or lining elements stone or stone-like materials, e.g. ceramics concrete; of glass or with an outer layer of stone or stone-like materials or glass
    • E04F13/142Coverings or linings, e.g. for walls or ceilings composed of covering or lining elements; Sub-structures therefor; Fastening means therefor composed of a plurality of similar covering or lining elements stone or stone-like materials, e.g. ceramics concrete; of glass or with an outer layer of stone or stone-like materials or glass with an outer layer of ceramics or clays
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B33/00Clay-wares
    • C04B33/02Preparing or treating the raw materials individually or as batches
    • C04B33/13Compounding ingredients
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    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B33/00Clay-wares
    • C04B33/02Preparing or treating the raw materials individually or as batches
    • C04B33/13Compounding ingredients
    • C04B33/132Waste materials; Refuse; Residues
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B33/00Clay-wares
    • C04B33/02Preparing or treating the raw materials individually or as batches
    • C04B33/13Compounding ingredients
    • C04B33/132Waste materials; Refuse; Residues
    • C04B33/1321Waste slurries, e.g. harbour sludge, industrial muds
    • C04B33/1322Red mud
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B33/00Clay-wares
    • C04B33/32Burning methods
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    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B38/00Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
    • C04B38/02Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by adding chemical blowing agents
    • EFIXED CONSTRUCTIONS
    • E04BUILDING
    • E04FFINISHING WORK ON BUILDINGS, e.g. STAIRS, FLOORS
    • E04F13/00Coverings or linings, e.g. for walls or ceilings
    • E04F13/07Coverings or linings, e.g. for walls or ceilings composed of covering or lining elements; Sub-structures therefor; Fastening means therefor
    • E04F13/072Coverings or linings, e.g. for walls or ceilings composed of covering or lining elements; Sub-structures therefor; Fastening means therefor composed of specially adapted, structured or shaped covering or lining elements
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3201Alkali metal oxides or oxide-forming salts thereof
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    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3205Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
    • C04B2235/3208Calcium oxide or oxide-forming salts thereof, e.g. lime
    • CCHEMISTRY; METALLURGY
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    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3262Manganese oxides, manganates, rhenium oxides or oxide-forming salts thereof, e.g. MnO
    • C04B2235/3267MnO2
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    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30Constituents and secondary phases not being of a fibrous nature
    • C04B2235/34Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3409Boron oxide, borates, boric acids, or oxide forming salts thereof, e.g. borax
    • CCHEMISTRY; METALLURGY
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    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30Constituents and secondary phases not being of a fibrous nature
    • C04B2235/44Metal salt constituents or additives chosen for the nature of the anions, e.g. hydrides or acetylacetonate
    • C04B2235/447Phosphates or phosphites, e.g. orthophosphate, hypophosphite
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/96Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P40/00Technologies relating to the processing of minerals
    • Y02P40/60Production of ceramic materials or ceramic elements, e.g. substitution of clay or shale by alternative raw materials, e.g. ashes

Abstract

The invention discloses a foamed ceramic material, a decorative plate and a preparation method, comprising the following steps: grinding the uniformly mixed raw materials to obtain mixed powder; carrying out water spraying granulation on the mixed powder to form granules; and filling the granules into a mould for sintering, and annealing after sintering to obtain the foamed ceramic material. The raw materials comprise: 10-60 parts of waste glass, 15-33 parts of red mud, 25-57 parts of coal gangue and 1-5 parts of foaming agent. The foamed ceramic material provided by the invention has the advantages of simple preparation process, low water absorption, small heat conductivity coefficient, good heat preservation performance and the like, the adopted raw materials have the advantages of wide sources, low price, industrial solid waste recycling and the like, in addition, the repeated recycling of materials can be realized in the production process, and the zero emission of waste materials is basically realized.

Description

Foamed ceramic material, decorative plate and preparation method
Technical Field
The invention relates to the technical field of comprehensive utilization of solid wastes and building materials, in particular to a foamed ceramic material, a decorative plate and a preparation method thereof.
Background
The coal gangue is solid waste generated in the coal mining process, the newly added coal gangue accounts for 3.7-6.6 hundred million tons each year in China, the yield is at the first position in the world, more than 1700 coal gangue mountains exist in China, and the accumulated stock amount reaches 45-50 million tons. If the coal gangue is not treated, the coal gangue is buried or stacked in the open air, not only a large amount of land is occupied, but also soil, rivers and underground water are polluted by harmful substances such as radioactive elements, heavy metals and polycyclic aromatic hydrocarbon compounds in the coal gangue, and harmful gases such as carbon dioxide, nitrogen oxides and sulfur dioxide released by spontaneous combustion of the coal gangue pollute the atmospheric environment and harm the human health. At present, the overall utilization rate of coal gangue in China is about 65%, wherein the coal gangue used for preparing building materials accounts for 12% of the total utilization amount, and the problem of recycling the coal gangue is urgently needed to be solved.
The foamed ceramic is a porous silicate material produced by a ceramic process, has high strength, light weight and small heat conductivity coefficient, and is used for various heat-insulating buildings and equipment. The raw materials used by the foamed ceramics are abundant, besides the common ceramic raw materials, tailing slag, television set disassembled glass, smelting waste residue, construction waste, and various silicate solid wastes such as shale, slate, coal gangue, fly ash and the like can be used as the raw materials of the foamed ceramics.
However, because the internal structure of the foamed ceramic is complex, closed holes which are uniformly distributed are difficult to form in the production process, which has adverse effects on the water absorption performance, the mechanical property, the heat conduction performance and the like of the foamed ceramic, and reduces the yield of the foamed ceramic; and the process for producing the ceramic has long process, is complex to operate, is difficult to control, is not beneficial to large-scale production, and greatly reduces the productivity. In addition, a large amount of residual leftover materials can be generated after the ceramic is subjected to a cutting process, so that the material waste is caused.
Disclosure of Invention
In view of the above-mentioned problems of the background art, the present invention provides a method for preparing a ceramic foam material, comprising:
grinding the uniformly mixed raw materials to obtain mixed powder;
carrying out water spraying granulation on the mixed powder to form granules;
filling the granules into a mould for sintering, and annealing after sintering to obtain the foamed ceramic material;
wherein the raw materials comprise: 10-60 parts of waste glass, 15-33 parts of red mud, 25-57 parts of coal gangue and 1-5 parts of foaming agent.
Further, the method for preparing the foamed ceramic material further comprises the following steps:
crushing 10-20 parts of vitrified tiles, mixing with the raw materials, and grinding to prepare the mixed powder; the particle size of the vitrified tile after being crushed is less than 0.088 mm.
Further, the granules are filled into a die for sintering, and after sintering, annealing is carried out to obtain the foamed ceramic material, wherein the foamed ceramic material comprises the following components:
filling the granules into a mould, heating to 500-550 ℃ at a heating rate of 3-10 ℃/min, and keeping the temperature for 30-40 min;
after the heat preservation is finished, the temperature is raised to 800-1000 ℃ at the temperature rise rate of 5-15 ℃/min, and the foaming is carried out for 50-70 min;
after foaming is finished, cooling to 550-650 ℃ according to the cooling rate of 10-30 ℃/min, and then naturally cooling to room temperature to obtain the foamed ceramic material.
Further, the total part of the waste glass, the red mud and the coal gangue is 100 parts.
Further, the raw materials also comprise a foam stabilizer and a fluxing agent; the foaming agent is selected from one or more of calcium carbonate, manganese dioxide and sodium silicate nonahydrate, the foam stabilizer is selected from trisodium phosphate and/or anhydrous sodium carbonate, and the fluxing agent is selected from borax and/or boric acid.
Further, the waste glass comprises 40 parts of coal gangue, 38 parts of red mud, 3 parts of manganese dioxide, 2 parts of borax and 2 parts of trisodium phosphate; the foaming temperature was 950 ℃.
Further, the particle size of the mixed powder is less than 0.088 mm.
The present invention also provides a foamed ceramic material prepared by any of the methods described above.
The volume weight of the foamed ceramic material is 0.55g/cm3-0.60g/cm3The compression strength is 1.0MPa-1.5MPa, and the volume water absorption is 4.3% -4.5%.
The invention also provides a decorative board which comprises the foamed ceramic material.
The foamed ceramic material provided by the invention has the advantages of simple preparation process, low water absorption, small heat conductivity coefficient, good heat preservation performance and the like, the adopted raw materials have the advantages of wide sources, low price, industrial solid waste recycling and the like, in addition, the repeated recycling of materials can be realized in the production process, and the zero emission of waste materials is basically realized.
Drawings
FIG. 1 is a flow chart of a process for preparing a foamed ceramic material according to the present invention;
FIG. 2 is a graph of the morphology and performance parameters of different raw material ratios, wherein (A) is a pore size morphology graph of the foamed ceramic prepared under the condition of different coal gangue mixing amounts, (B) is a volume-weight curve graph of the foamed ceramic under the condition of different coal gangue mixing amounts, and (C) is a water absorption curve graph of the foamed ceramic under the condition of different coal gangue mixing amounts;
FIG. 3 is a graph of the appearance and performance parameters of different foaming temperatures, wherein (A) is a pore size appearance graph of the coal gangue foam ceramic prepared under different foaming temperatures, (B) is a graph of the influence of different foaming temperatures on the bulk density of the coal gangue foam ceramic, and (C) is a graph of the influence of different foaming temperatures on the water absorption of the coal gangue foam ceramic;
FIG. 4 is a graph of the morphology and performance parameters of different foaming holding times, wherein (A) is a pore size morphology graph of the coal gangue foam ceramic under different foaming times, (B) is a graph of the influence of different foaming times on the volume weight of the coal gangue foam ceramic, and (C) is a graph of the influence of different foaming times on the water absorption of the coal gangue foam ceramic;
FIG. 5 is a graph of the morphology and performance parameters of various blowing agents and levels, where (A) is CaCO as the blowing agent3The pore diameter appearance figure of the prepared foamed ceramic is shown in the specification, and (B) the foaming agent is MnO2The pore diameter appearance graph of the prepared foamed ceramic is shown in the specification, and (C) the foaming agent is Na2SiO4·9H2The pore diameter appearance graph of the foamed ceramic prepared at O time, (D) is a curve chart of the influence of different foaming agents and contents on the volume weight of the foamed ceramic, and (E) is a curve chart of different foaming agents and contentsA graph of the effect on the water absorption of the ceramic foam;
FIG. 6 is a graph of the morphology and performance parameters of various foam stabilizers and amounts thereof, wherein (A) is Na as the foam stabilizer3PO4The pore diameter appearance of the prepared foam ceramic is shown in the figure, and (B) the foam stabilizer is anhydrous Na2CO3The pore size appearance of the prepared foam ceramic, (C) is a curve graph of the influence of different foam stabilizers and contents on the volume weight of the foam ceramic, and (D) is a curve graph of the influence of different foam stabilizers and contents on the water absorption of the foam ceramic;
FIG. 7 is a graph of the morphology and performance parameters of various fluxing agents and contents, wherein (A) is a pore size morphology of the ceramic foam prepared with borax as a fluxing agent, (B) is a pore size morphology of the ceramic foam prepared with boric acid as a fluxing agent, (C) is a graph of the effect of various fluxing agents and contents on the bulk weight of the ceramic foam, and (D) is a graph of the effect of various fluxing agents and contents on the water absorption of the ceramic foam.
Detailed Description
The technical solutions in the embodiments of the present application will be clearly and completely described below, and it should be apparent that the described embodiments are some, but not all, embodiments of the present application. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present application.
The terms "including" and "having," as well as any variations thereof, are intended to cover non-exclusive inclusions. For example, a process, method, system, article, or apparatus that comprises a list of steps or elements is not limited to only those steps or elements listed, but may alternatively include other steps or elements not listed, or inherent to such process, method, article, or apparatus.
Reference herein to "an embodiment" means that a particular feature, structure, or characteristic described in connection with the embodiment can be included in at least one embodiment of the application. The appearances of the phrase in various places in the specification are not necessarily all referring to the same embodiment, nor are separate or alternative embodiments mutually exclusive of other embodiments. It is explicitly and implicitly understood by one skilled in the art that the embodiments described herein can be combined with other embodiments.
Fig. 1 shows a method for preparing a foamed ceramic material provided by the present invention, specifically, the method comprises:
grinding the uniformly mixed raw materials to obtain mixed powder;
carrying out water spraying granulation on the mixed powder to form granules;
and filling the granules into a mould for sintering, and annealing after sintering to obtain the foamed ceramic material.
Wherein the raw materials comprise 10-60 parts of waste glass, 15-33 parts of red mud, 25-57 parts of coal gangue and 1-5 parts of foaming agent.
The waste glass is a waste beer bottle, and table 1 shows the chemical composition of one waste glass usable in the present invention.
Table 1 main chemical composition and content (%)
Red mud is an industrial solid waste produced after alumina is extracted from bauxite. Table 2 shows the chemical composition of one of the red mud used in the present invention.
Table 2 main chemical composition and content (%) -of red mud
The coal gangue mainly contains silicon, aluminum, iron and other elements, and the coal gangue contains more kaolinite (Al)2O3·2SiO2·2H2O) and Quartz (SiO)2). Table 3 shows the chemical composition of a coal refuse usable in the present invention.
TABLE 3 Main chemical composition and content (%)
Further, the raw materials also comprise a foam stabilizer and a fluxing agent. The foaming agent is selected from one or more of calcium carbonate, manganese dioxide and sodium silicate nonahydrate.
Further, the foamed ceramic material may further include a foam stabilizer and/or a flux. The foam stabilizer is selected from trisodium phosphate and/or anhydrous sodium carbonate. The fluxing agent is selected from borax and/or boric acid.
Further, the method for preparing the foamed ceramic material further comprises the following steps:
crushing 10-20 parts of vitrified tiles, mixing with the raw materials, and grinding to prepare the mixed powder; the particle size of the vitrified tile after being crushed is less than 0.088 mm.
The vitrified tiles are waste tiles and table 4 shows the chemical composition of one vitrified tile that can be used in the present invention.
TABLE 4 vitrified tiles Main chemical composition (%)
The vitrified tile is added into the ingredient mixing procedure in the form of raw materials and is recycled. The waste ceramic tiles sintered at high temperature have high activity, can play a positive role in the subsequent firing process, and have good inspection effect. Meanwhile, the operation mode can achieve the purpose of recycling materials, and basically realizes zero emission of waste materials.
Optionally, the particle size of the mixed powder is less than 0.080 mm.
Optionally, before mixing the raw materials, the raw materials are respectively pretreated in the following specific manner:
(1) glass: washing waste glass with clear water, naturally drying, crushing to 3-5cm, and ball milling the glass fragments in a conical ball mill. The ball-material ratio is 10:1, 1.5kg of glass is ground by ball milling each time, 15kg of grinding balls are added, and the ball milling time is 20 min. After ball milling, the glass powder firstly passes through a standard sieve with the aperture of 20 meshes (the aperture is 1.0mm), large-particle powder is sieved out, and then the glass fine powder passes through a standard sieve with the aperture of 180 meshes (the aperture is 0.088 mm);
(2) red mud: drying the red mud in a constant-temperature oven at 105 ℃ for 5 hours, and then putting the red mud into a conical ball mill for ball milling. The ball-material ratio is 10:1, the ball-milling sample is 1.5kg each time, 15kg of grinding balls are added, the ball-milling time is 20min, and the red mud powder directly passes through a 180-mesh standard sieve (the aperture is 0.088 mm).
(3) Coal gangue: firstly, crushing the coal gangue to 1-2cm by a jaw crusher, and then putting the coal gangue into a conical ball mill for ball milling. The ball-material ratio is 10:1, the coal gangue is milled by 1.5kg each time, the grinding balls are added by 15kg, and the ball milling time is 20 min. After ball milling, the coal gangue powder firstly passes through a standard sieve with the aperture of 20 meshes (the aperture is 1.0mm), large particle powder is sieved out, and then the coal gangue fine powder passes through a standard sieve with the aperture of 180 meshes (the aperture is 0.088 mm).
(4) And (3) vitrified brick: washing the vitrified tile with clear water, naturally drying, crushing the vitrified tile by a jaw crusher, and then putting the vitrified tile into a conical ball mill for ball milling. Adding 15kg of grinding balls and 1.5kg of vitrified tiles, and performing ball milling for 30 min. And (3) screening large-particle powder by a standard sieve with the aperture of 1.0mm and screening fine powder by a standard sieve with the aperture of 0.088mm after ball milling to obtain vitrified tile powder.
Optionally, filling the granules into a mold, and then heating to 500-550 ℃ at a heating rate of 3-10 ℃/min, wherein the heat preservation time is 30-40 min; after the heat preservation is finished, the temperature is raised to 800-1000 ℃ at the temperature rise rate of 5-15 ℃/min, and the foaming is carried out for 50-70 min; after foaming is finished, cooling to 550-650 ℃ according to the cooling rate of 10-30 ℃/min, and then naturally cooling to room temperature to obtain the foamed ceramic material.
The foamed ceramics prepared by the method are subjected to structural characterization and the following performance tests:
(1) structural characterization:
the phase analysis of the foamed ceramic was carried out using an X' Pert pro powder X-ray diffractometer (XRD) of the Pasnake, Netherlands, and the chemical composition of the material was analyzed using a Nippon-science Wisdom-6000X-ray fluorescence spectrometer (XRF).
(2) Topography observation
The test mainly observes and records the overall foaming effect of the sample, the pore size of the pores, the distribution condition of the pores, the thickness of the pore walls and other morphological characteristics, and takes pictures through a mobile phone to carry out comparative analysis.
(3) Volume weight
The volume weight was tested according to GB/T1966-.
(4) Water absorption rate
Testing of Water absorption: weighing a sample taken out of a high-temperature furnace to obtain m1, placing the sample into water, standing for 2h, taking out the sample, wiping the surface moisture with a towel, wiping the surface of the sample with absorbent paper twice, and removing the surface moisture; finally, the mass m2 of the sample after water absorption was measured. The water absorption of the sample is (m2-m1)/m 1.
(5) Compressive strength
Sawing the upper surface and the lower surface of the sample into flat surfaces, putting the sample in a pressure testing machine to be pressed down until the sample is damaged, reading the reading on the pressure testing machine, and dividing the reading by the area of the test piece to obtain the compressive strength of the test piece.
The raw materials used in the examples:
waste glass: glass of Qingdao and Laoshan beer bottles;
and (3) vitrified brick: the vitrified tiles discarded in the flat mountain building material market;
calcium carbonate: analytical purity, Tianjin Bodi chemical corporation;
manganese dioxide: analytical purity, Tianjin Bodi chemical corporation;
sodium silicate nonahydrate: analytical purity, Tianjin Bodi chemical corporation;
trisodium phosphate: analytical purity, Tianjin Bodi chemical corporation;
anhydrous sodium carbonate: analytically pure, chemical reagent factory of Luoyang city;
borax: analytical purity, Tianjin Bodi chemical corporation;
boric acid: analytical purity, Henjin chemical reagents manufacturing Co., Ltd.
Example 1
1. Determining the raw material proportion of the foamed ceramics
The foamed ceramic comprises 10 parts of waste glass, 20 parts of waste glass, 30 parts of waste glass, 40 parts of waste glass, 50 parts of waste glass and 60 parts of coal gangue, 25 parts of coal gangue, 32 parts of coal gangue, 38 parts of coal gangue, 44 parts of coal gangue, 51 parts of coal gangue and 57 parts of coal gangue, wherein the mass sum of the waste glass, the coal gangue and the red mud is 100 parts. The foaming agent is calcium carbonate, and the calcium carbonate accounts for 3 parts; trisodium phosphate is selected as the foam stabilizer, borax is selected as the fluxing agent, and the content is 2 parts. The foaming temperature was determined to be 950 ℃ and the foaming time 60 min. The ceramic foam formulation is shown in Table 5 and the results are shown in FIG. 2.
TABLE 5 foamed ceramics recipe (parts)
From fig. 2(a), it can be derived that: when the coal gangue content is lower, the pores are less, the pore diameter is larger, and the distribution is uneven, from the macroscopic structure, when the coal gangue content is 32 parts, the pores are relatively uniformly distributed, but the pore diameter ratio is larger, and when the coal gangue content is 38 parts and 44 parts, the corresponding pore sizes and the distribution of the foamed ceramics are relatively uniform. Therefore, the corresponding mixing ratio is an appropriate mixing ratio when the coal gangue content is 38 parts and 44 parts.
As shown in FIG. 2B, the volume weight of the foamed ceramic decreases first and then increases with the increase of the coal gangue content, and when the coal gangue content is 38 parts, the volume weight is the smallest, which is about 0.52g/cm3. Generally, the smaller the volume weight, the greater the corresponding porosity. Therefore, the preferable contents determined by volume weight are 40 parts of waste glass, 38 parts of coal gangue and 22 parts of red mud.
As shown in fig. 2(C), as the coal gangue content increases, the water absorption rate of the ceramic foam increases and then decreases. The larger the water absorption, the more open pores capable of adsorbing free water. Accordingly, the proper coal gangue content is determined to be 38 parts.
According to the analysis of the distribution of macroscopic pores of the foamed ceramic, the pore size, the volume weight and the water absorption rate, the preferable mixing ratio is as follows: 40 parts of waste glass, 38 parts of coal gangue and 22 parts of red mud.
2. Determining the foaming temperature of a ceramic foam
The mixture ratio is determined as 40 portions of waste glass, 38 portions of coal gangue, 22 portions of red mud, 3 portions of calcium carbonate, and 2 portions of trisodium phosphate and borax. The foaming time was 60min, the foaming temperature was 800 deg.C, 850 deg.C, 900 deg.C, 950 deg.C and 1000 deg.C, respectively, as shown in Table 6, and the results are shown in FIG. 3.
TABLE 6 foaming temperature protocol
As can be seen from FIG. 3(A), under the condition of the same coal gangue content, the foaming condition of the ceramic is not ideal below 900 ℃, and the foamed ceramic has better foaming effect and more uniform distribution of pores at 950 ℃ and 1000 ℃. Therefore, from the morphology of the pores, 950 ℃ and 1000 ℃ are more suitable foaming temperatures.
As shown in FIG. 3(B), the volume weight of the ceramic foam decreases and then increases with the increase of the foaming temperature, and the volume weight is the lowest at 950 ℃ and is about 0.52g/cm3This indicates that the porosity of the ceramic foam is large under this temperature condition.
In FIG. 3C, the water absorption rate of the ceramic foam increases and then decreases as the foaming temperature increases, and the water absorption rate becomes maximum at a foaming temperature of 950 ℃, which shows that the ceramic foam fired at this temperature has many open pores capable of adsorbing free water.
Comprehensively considering the pore formation condition, the volume weight and the water absorption rate of the coal gangue foam ceramic, the preferable foaming temperature of the coal gangue foam ceramic is 950 ℃.
3. Determining the foaming holding time of the foamed ceramic
The mixture ratio is determined as 40 parts of waste glass, 38 parts of coal gangue, 22 parts of red mud, 3 parts of calcium carbonate, 2 parts of trisodium phosphate and borax, the foaming temperature is 950 ℃, the foaming time is 30min, 60min and 90min, see table 7, and the result is shown in figure 4.
TABLE 7 foaming incubation time protocol
As shown in fig. 4, the mixture ratio is 40 parts of waste glass, 38 parts of coal gangue and 22 parts of red mud, when the foaming temperature is 950 ℃, more bubbles are generated in different foaming time, but in the foaming time of 30min and 90min, the pore diameter and distribution uniformity of the bubbles of the foamed ceramic are poor, and when the foaming time is 60min, the pore diameter and distribution are uniform compared with the other two foaming time, so 60min is selected as the better sintering foaming time of the foamed ceramic.
When the foaming time is 30min, the ceramic is not fully foamed, and the volume weight is about 1.58g/cm3When the foaming time is 90min, the ceramic firing time is too long, the liquid phase is too much, and pores formed earlier are filled, so that the volume weight is larger than that of the ceramic when the foaming time is 60 min. Therefore, the temporary setting of 60min is the preferable foaming temperature of the foamed ceramic.
When the foaming time is 60min, the water absorption of the foamed ceramic reaches the maximum, which shows that the foamed ceramic fired at the foaming time can absorb more open pores of free water.
Through comprehensive analysis of three groups of experimental results, the optimal foaming time of the foamed ceramic should be selected to be 60 min.
4. Determination of foaming agent of foamed ceramic
The mixture ratio is determined as 40 portions of waste glass, 38 portions of coal gangue and 22 portions of red mud, 2 portions of trisodium phosphate and borax, the foaming temperature is 950 ℃, the foaming time is 60min, and the foaming agent is CaCO respectively3、MnO2And Na2SiO4·9H2O, in amounts of 2 parts, 3 parts, 4 parts, 5 parts and 6 parts, respectively, are shown in Table 8, and the results are shown in FIG. 5.
TABLE 8 ingredient composition (parts) of sample
As can be seen from FIG. 5, CaCO is incorporated3The foam ceramic has better internal foaming effect along with CaCO3The content is increased gradually, the pore diameter of the pores in the foamed ceramic is increased, and the pore wall is thinned. With MnO2The content is increased gradually, so that the pore diameter of the pores in the foamed ceramic is increased, and the pore walls are thinned. When the content is 3 parts, the pore diameter is about 3mm, and the size and the distribution are uniform. Na (Na)2SiO4·9H2Content of OWhen the shape, the size and the distribution of the internal pores of the foamed ceramics are changed greatly. Na (Na)2SiO4·9H2When the content of O is 2 parts, the foaming inside the foamed ceramic is relatively uniform, but the pore size is small and the distribution is dense. The volume weight of the foamed ceramic is gradually reduced along with the increasing of the content of the foaming agent, because the amount of the reaction decomposed gas is increased along with the increasing of the content, the gas pressure in the pores is increased sharply, and the volume of the prepared sample is increased and the volume weight is reduced due to the larger foaming pores.
With CaCO3And MnO2In the case of a foaming agent, the bulk weight is relatively low, Na2SiO49H2O is a blowing agent, the bulk density is higher than in the other two cases. Comparison of the three blowing agents, CaCO3At 6 parts, the volume weight of the ceramic foam is minimum, about 0.38g/cm3
With CaCO3Or MnO2In the case of the foaming agent, the water absorption rate gradually increases with increasing content. With CaCO3For the blowing agent, the contents were 2 parts, 3 parts and 4 parts, the water absorption rate was almost unchanged, but the volume weight was decreased, indicating that the total porosity was increasing, but the open pore porosity was not greatly different, and the closed pore porosity was gradually increased with the increase in the blowing agent content.
With Na2SiO4·9H2When O is a blowing agent, the water absorption decreases as the blowing agent content increases, and the volume weight also decreases gradually as the blowing agent content increases. Description of the use of Na2SiO4·9H2At O, the pores formed by foaming are mostly closed pores.
5. Foam stabilizer for determining foamed ceramics
The mixture ratio is determined as 40 portions of waste glass, 38 portions of coal gangue, 22 portions of red mud, 3 portions of manganese dioxide, 2 portions of borax, the foaming temperature is 950 ℃, the foaming time is 60min, and the foam stabilizer contains Na3PO4And anhydrous sodium carbonate in amounts of 1 part, 2 parts, 3 parts, 4 parts, and 5 parts, respectively, as shown in Table 9, and the results are shown in FIG. 6.
TABLE 9 ingredient composition (parts) of sample
As can be seen from FIG. 6, Na is used3PO4When the foam stabilizer is used, the foam stabilizing effect is relatively remarkable at each content, and the whole sample has good foaming, high content and large pores. When the content is 2 parts, the pore size and the distribution are uniform. The foam stabilizing effect of each content is poor, the surface of the sample is partially peeled off, the edge is caked, the internal pore diameter is irregular, most of the pore diameters are smaller, and the pore wall is thicker.
With Na3PO4In the case of the foam stabilizer, the volume weight tends to decrease gradually as the content increases. When the content is 5 parts, the volume weight is the smallest, and is reduced by about 14 parts compared with the content of 1 part.
With anhydrous Na2CO3In the case of foam stabilizer, the volume weight is gradually reduced along with the increasing content, and when the content is 4 parts, the volume weight is the lowest and is about 0.45g/cm3And the content is reduced by about 29 parts compared with 1 part.
With Na3PO4In the case of the foam stabilizer, the water absorption rate gradually decreases with increasing content, which means that the open pore porosity decreases and more closed pores are formed. With anhydrous Na2CO3In the case of the foam stabilizer, the water absorption rate increases with increasing content, because anhydrous sodium carbonate generates CO under high temperature condition2Gas, more open pores are formed.
6. Flux for determining ceramic foam
The compounding ratio is determined as 40 parts of waste glass, 38 parts of coal gangue, 22 parts of red mud, 3 parts of manganese dioxide, 2 parts of trisodium phosphate, the foaming temperature is 950 ℃, the foaming time is 60min, the fluxing agents are borax and boric acid, the adding amount is 1 part, 2 parts, 3 parts, 4 parts and 5 parts respectively, see table 10, and the result is shown in figure 7.
Ingredient composition (parts) of the sample in Table 10
As can be seen from fig. 7, the pore size gradually increased with increasing borax content. When the content of borax is 2 parts, the aperture size is proper, but when the content is 3 parts, 4 parts and 5 parts, the fluxing effect is too obvious, and the hole wall around the macropore is thicker. The boric acid with various contents has large and small holes on the sample, the higher the content is, the whole forming of the sample is unstable, the bubbles are not uniform, and the fluxing effect is poor.
The bulk weight of the sample gradually decreases as the flux content increases. Compared with the same content, the volume weight of the foamed ceramic is slightly lower when the borax is doped; when the adding amount is 5 parts, the volume weight of the foamed ceramic added with the boric acid is slightly lower. 5 parts of boric acid fluxing agent is added, and the volume weight of the foamed ceramic is about 0.49g/cm3
The water absorption of the test piece gradually increases with the increasing content of the fluxing agent. Compared with the same content, the foamed ceramic has relatively larger water absorption when the boric acid is mixed.
Example 2
The foamed ceramic material is prepared from 40 parts of waste glass, 38 parts of coal gangue, 22 parts of red mud, 3 parts of manganese dioxide, 2 parts of borax and 2 parts of trisodium phosphate.
The preparation process of the foamed ceramic material comprises the following steps:
the raw materials are respectively crushed and ground to ensure that the particle size is less than 0.088 mm. Then, the materials are weighed and mixed according to the proportion to obtain uniformly mixed powder, and then grinding is carried out, wherein the particle size of the mixed powder is less than 0.088 mm. And carrying out water spraying granulation on the mixed powder to form granules, wherein the amount of water spraying is 5% of the mass of the mixed raw materials. Then placing the mixture into a refractory silicon carbide mould, compacting the refractory silicon carbide mould, and then sending the compacted refractory silicon carbide mould into a roller kiln for firing. Preheating is carried out firstly, the temperature is raised to 500 ℃ from the initial temperature, the preheating temperature rise rate is 7 ℃/min, and when the temperature reaches 500 ℃, the temperature is kept for 30 min. Then heating to foaming temperature from 500 ℃, wherein the heating rate of sintering foaming is 9 ℃/min, the foaming temperature is 950 ℃, and foaming is carried out for 60min when the foaming temperature is reached. And (3) after the firing period is finished, entering an annealing and cooling program, rapidly cooling from the foaming temperature to 600 ℃ to be a cooling stage, wherein the cooling rate is 20 ℃/min, naturally cooling from 600 ℃ to room temperature, and the annealing time is 18 h.
The performance of the foamed ceramic product is detected, and the volume weight is 0.57g/cm3The compressive strength was 1.3MPa, and the volume water absorption rate is 4.4 percent.
Example 3
The foamed ceramic material is prepared from 40 parts of waste glass, 38 parts of coal gangue, 22 parts of red mud, 15 parts of vitrified tiles, 3 parts of manganese dioxide, 2 parts of borax and 2 parts of trisodium phosphate.
The preparation process of the foamed ceramic material comprises the following steps:
the raw materials are respectively crushed and ground to ensure that the particle size is less than 0.088 mm. Then, the materials are weighed and mixed according to the proportion to obtain uniformly mixed powder, and then grinding is carried out, wherein the particle size of the mixed powder is less than 0.088 mm. And carrying out water spraying granulation on the mixed powder to form granules, wherein the amount of water spraying is 5% of the mass of the mixed raw materials. Then placing the mixture into a refractory silicon carbide mould, compacting the refractory silicon carbide mould, and then sending the compacted refractory silicon carbide mould into a roller kiln for firing. Preheating is carried out firstly, the temperature is raised to 500 ℃ from the initial temperature, the preheating temperature rise rate is 7 ℃/min, and when the temperature reaches 500 ℃, the temperature is kept for 30 min. Then heating to foaming temperature from 500 ℃, wherein the heating rate of sintering foaming is 9 ℃/min, the foaming temperature is 950 ℃, and foaming is carried out for 60min when the foaming temperature is reached. And (3) after the firing period is finished, entering an annealing and cooling program, rapidly cooling from the foaming temperature to 600 ℃ to be a cooling stage, wherein the cooling rate is 20 ℃/min, naturally cooling from 600 ℃ to room temperature, and the annealing time is 18 h.
The performance of the foamed ceramic product is detected, and the volume weight is 0.57g/cm3The compressive strength is 1.5MPa, and the volume water absorption is 4.4%.
Example 4
Preparing a decorative plate, wherein the waste glass comprises 40 parts, 38 parts of coal gangue, 22 parts of red mud, 15 parts of vitrified tiles, 3 parts of manganese dioxide, 2 parts of borax and 2 parts of trisodium phosphate.
The preparation process of the decorative plate comprises the following steps:
the raw materials are respectively crushed and ground to ensure that the particle size is less than 0.088 mm. Then, the raw materials are weighed respectively according to the proportion and then mixed to obtain uniformly mixed powder, and then grinding is carried out, wherein the particle size of the mixed powder is smaller than 0.088 mm. And carrying out water spraying granulation on the mixed powder to form granules, wherein the amount of water spraying is 5% of the mass of the mixed raw materials. Then placing the mixture into a refractory silicon carbide mould, compacting the refractory silicon carbide mould, and then sending the compacted refractory silicon carbide mould into a roller kiln for firing. Preheating is carried out firstly, the temperature is raised to 500 ℃ from the initial temperature, the preheating temperature rise rate is 7 ℃/min, and when the temperature reaches 500 ℃, the temperature is kept for 30 min. Then heating to foaming temperature from 500 ℃, wherein the heating rate of sintering foaming is 9 ℃/min, the foaming temperature is 950 ℃, and foaming is carried out for 60min when the foaming temperature is reached. And (3) after the firing period is finished, entering an annealing and cooling program, rapidly cooling from the foaming temperature to 600 ℃ to be a cooling stage, wherein the cooling rate is 20 ℃/min, naturally cooling from 600 ℃ to room temperature, and the annealing time is 18 h. The foamed ceramic material prepared above was cut in a mold equipped with a ceramic fiber paper liner.
In the embodiment, the original mold size is changed from 1.6m × 1.6.6 m × 0.2.2 m to 1.6m × 3.1.1 m × 0.32.32 m, so that each m is equal to3The ceramic fiber paper lining the die used for the finished product is 10.11m2Reduced to 6.09m2. The yield of the material is improved from 75% to 85%, and the whole process productivity is improved by 66%.
The foamed ceramic material provided by the invention has the advantages of simple preparation process, low water absorption, small heat conductivity coefficient, good heat preservation performance and the like, the adopted raw materials have the advantages of wide sources, low price, industrial solid waste recycling and the like, in addition, the repeated recycling of materials can be realized in the production process, and the zero emission of waste materials is basically realized.
It should be noted that the above-mentioned embodiments are only examples of the present invention, and not intended to limit the scope of the present invention, and all changes of equivalent structures and equivalent processes, such as mutual combination of technical features between various embodiments, or direct or indirect application to other related technical fields, which are made by the present specification, are included in the scope of the present invention.

Claims (10)

1. A method of preparing a ceramic foam material, comprising:
grinding the uniformly mixed raw materials to obtain mixed powder;
carrying out water spraying granulation on the mixed powder to form granules;
filling the granules into a mould for sintering, and annealing after sintering to obtain the foamed ceramic material;
wherein the raw materials comprise: 10-60 parts of waste glass, 15-33 parts of red mud, 25-57 parts of coal gangue and 1-5 parts of foaming agent.
2. The method of claim 1, further comprising:
crushing 10-20 parts of vitrified tiles, mixing with the raw materials, and grinding to prepare the mixed powder; the particle size of the vitrified tile after being crushed is less than 0.088 mm.
3. The method of claim 1, wherein the step of filling the pellets into a mold for sintering, and the step of annealing after the sintering step to obtain the foamed ceramic material comprises:
filling the granules into a mould, heating to 500-550 ℃ at a heating rate of 3-10 ℃/min, and keeping the temperature for 30-40 min;
after the heat preservation is finished, the temperature is raised to 800-1000 ℃ at the temperature rise rate of 5-15 ℃/min, and the foaming is carried out for 50-70 min;
after foaming is finished, cooling to 550-650 ℃ according to the cooling rate of 10-30 ℃/min, and then naturally cooling to room temperature to obtain the foamed ceramic material.
4. The method according to claim 1, wherein the total part of the waste glass, the red mud and the coal gangue is 100 parts.
5. The method of claim 1, wherein the raw materials further comprise a foam stabilizer and a fluxing agent; the foaming agent is selected from one or more of calcium carbonate, manganese dioxide and sodium silicate nonahydrate, the foam stabilizer is selected from trisodium phosphate and/or anhydrous sodium carbonate, and the fluxing agent is selected from borax and/or boric acid.
6. The method according to any one of claims 1 to 5, wherein the waste glass comprises 40 parts, 38 parts of coal gangue, 22 parts of red mud, 3 parts of manganese dioxide, 2 parts of borax and 2 parts of trisodium phosphate; the foaming temperature was 950 ℃.
7. The method of claim 1, wherein the particle size of the powder blend is less than 0.088 mm.
8. A foamed ceramic material prepared by the process of any one of claims 1-7.
9. The foamed ceramic material of claim 8, wherein the foamed ceramic material has a volume weight of 0.55g/cm3-0.60g/cm3The compression strength is 1.0MPa-1.5MPa, and the volume water absorption is 4.3% -4.5%.
10. A decorative panel comprising the ceramic foam material of claim 8 or 9.
CN202010687847.7A 2020-07-16 2020-07-16 Foamed ceramic material, decorative plate and preparation method Pending CN111747725A (en)

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