CN116903386A - Preparation method of fly ash-based honeycomb ceramic - Google Patents

Preparation method of fly ash-based honeycomb ceramic Download PDF

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CN116903386A
CN116903386A CN202310671922.4A CN202310671922A CN116903386A CN 116903386 A CN116903386 A CN 116903386A CN 202310671922 A CN202310671922 A CN 202310671922A CN 116903386 A CN116903386 A CN 116903386A
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fly ash
mud
blank
honeycomb ceramic
drying
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陈燚
杨宇
冯宏
洪钦
胡一鸣
李明
朱伟
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Tongxiang Tai Aisi Environmental Energy Co ltd
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    • C04B38/00Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
    • C04B38/0006Honeycomb structures
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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
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    • C04B33/00Clay-wares
    • C04B33/02Preparing or treating the raw materials individually or as batches
    • C04B33/13Compounding ingredients
    • C04B33/1315Non-ceramic binders
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    • C04B33/00Clay-wares
    • C04B33/02Preparing or treating the raw materials individually or as batches
    • C04B33/13Compounding ingredients
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    • C04B33/00Clay-wares
    • C04B33/02Preparing or treating the raw materials individually or as batches
    • C04B33/13Compounding ingredients
    • C04B33/132Waste materials; Refuse; Residues
    • C04B33/135Combustion residues, e.g. fly ash, incineration waste
    • C04B33/1352Fuel ashes, e.g. fly ash
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    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/63Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
    • C04B35/632Organic additives
    • C04B35/636Polysaccharides or derivatives thereof
    • C04B35/6365Cellulose or derivatives thereof
    • 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
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    • 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 preparation method of fly ash-based honeycomb ceramics, and belongs to the technical field of inorganic nonmetallic materials. The method comprises the following steps: ball milling and drying fly ash, preparing a mud blank, vacuum mud refining, ageing the mud blank, vacuum extrusion molding, microwave shaping, drying by a baking oven, high-temperature sintering and processing by a through hole. The fly ash-based honeycomb ceramic produced by the formula and the process has excellent acid and alkali resistance, high thermal stability and thermal expansion coefficient lower than 1.0 x 10 ‑6 and/C. The honeycomb ceramic has the following advantages: the chemical stability is good, and acid and alkali resistance and organic solvent are realized; excellent rapid heat quenching resistancePerformance, working temperature can reach more than 1000 ℃; the antibacterial property is good, and the antibacterial agent is not easy to degrade by bacteria; the method has the advantages of strong structural stability, low preparation cost, simple and convenient operation method, no environmental pollution and the like, and provides a feasible high-value resource utilization way for the coal-fired fly ash.

Description

Preparation method of fly ash-based honeycomb ceramic
Technical Field
The invention relates to the technical field of inorganic nonmetallic materials, in particular to a preparation method of fly ash-based honeycomb ceramics.
Background
Honeycomb ceramics have been developed over the last three decades as a new ceramic product with a honeycomb-like structure consisting of a multitude of parallel straight channels. Because of the characteristics of multiple hollow thin walls, compared with other materials, the catalyst has the advantages of larger specific surface area, good strength and the like, can lead the gas-liquid distribution to be more uniform, has small bed resistance and long service life, and is widely applied to industrial processes such as chemical industry, electric power, metallurgy, petroleum, electronic appliances, machinery and the like from the earliest use in purifying the tail gas of a small automobile. The honeycomb ceramics can be made of various materials, and the main materials are as follows: composite matrixes such as cordierite, mullite, aluminum titanate, activated carbon, silicon carbide, activated alumina, zirconia, silicon nitride, cordierite-mullite, cordierite-aluminum titanate and the like.
Fly ash produced by a coal-fired thermal power plant is the largest single solid waste in China at present. The annual production of the Chinese fly ash in 2020 reaches 6.5 hundred million tons, and the accumulation amount is increased year by year and exceeds 30 hundred million tons due to the huge production amount for a long time and difficult complete consumption. Fly ash in the form of fine powder is easy to drift along with wind, and has great harm to air, water source and soil, and seriously threatens natural environment and human health. The main component of the fly ash is SiO 2 And Al 2 O 3 The sum of the contents of the components is generally more than 50% of the chemical composition, and the content of the components in the high-alumina fly ash can be up to more than 70%, so that the high-alumina fly ash is a potential aluminosilicate mineral material. The coal ash has smooth spherical micro beads as the micro morphology, and has partial porous particles, complicated structure particles, irregular large particles, scraps and the like, and the particle size is generally 1-100 mu m. The chemical components of the composite material and cordierite and mullite areThe similarity, fine grain diameter and good stability, is a high-quality honeycomb ceramic raw material. The preparation of the honeycomb ceramics by using the surplus fly ash not only can realize the reutilization of resources, but also can provide a feasible way for the treatment and disposal of the fly ash, and ensure the stable operation of a power plant.
Disclosure of Invention
The invention aims to provide a preparation method of fly ash-based honeycomb ceramics, which has the advantages of low preparation cost, simple and convenient operation and no environmental pollution; the prepared honeycomb ceramic has strong structural stability, excellent acid and alkali resistance, high thermal stability and low thermal expansion coefficient.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
the preparation method of the fly ash-based honeycomb ceramic takes fly ash as a raw material to prepare the honeycomb ceramic, and specifically comprises the following steps:
(1) Preparing a ceramic mud blank: mixing fly ash, binder solution and lubricant in a mud mixer to obtain ceramic mud blank; the method comprises the steps of carrying out a first treatment on the surface of the Wherein the weight of the binder solution is 20-35 wt.% of the weight of the fly ash, and the weight of the lubricant is 2-5 wt.% of the weight of the fly ash;
(2) Performing vacuum mud refining and mud blank aging treatment on the ceramic mud blank obtained in the step (1);
(3) Carrying out vacuum extrusion on the mud blank subjected to the ageing treatment in the step (2) to obtain a fly ash-based honeycomb ceramic wet blank with the required pore density;
(4) Immediately cutting the wet blank by using a stainless steel wire to a required length after vacuum extrusion, rapidly putting the wet blank into a microwave oven for microwave shaping, and drying the microwave shaping, wherein the microwave shaping is carried out by using high fire for 5min; drying in an oven after microwave shaping, naturally cooling, and processing the end face of the dried honeycomb ceramic to obtain a honeycomb ceramic blank with a neat end face;
(5) And (3) placing the honeycomb ceramic blank with the neat end face obtained after the treatment in the step (4) into a muffle furnace for high-temperature sintering and pore canal treatment, and obtaining the fly ash-based honeycomb ceramic.
The raw material fly ash used in the invention is solid waste formed by high-temperature combustion of coal fuel of a coal-fired power plant, is homogeneous powder, and has the particle size of 1-100 mu m.
The raw material fly ash is subjected to pretreatment before being used, wherein the pretreatment is ball milling, drying and sieving treatment which are sequentially carried out; the ball milling treatment process comprises the following steps: according to the proportion of adding 1-2 kg of deionized water into each kg of raw material fly ash, adding neutral dispersant JA282 accounting for 0.1-3 wt.% of the weight of the fly ash, and carrying out wet ball milling mixing by using a roller ball mill, wherein the ball-to-material ratio is 1:1 to 3:1, ball milling time is 5-20 h; the drying treatment process comprises the following steps: drying the ball-milled discharge in an oven at 50-200 ℃ for 24-48 h to obtain uniformly mixed and dried fly ash raw material powder; the sieving treatment is to naturally cool the pulverized coal ash powder after ball milling and drying in a baking oven, and then directly pass through a 120-mesh screen, wherein the upper part of the screen is further crushed and then is continuously sieved.
In the step (1), the binder solution is prepared by dissolving a binder in water to prepare a binder solution with the concentration of 10-35 wt.%, wherein the binder is methyl cellulose, hydroxypropyl methyl cellulose or hydroxyethyl methyl cellulose; the lubricant is vegetable oil, paraffin emulsion or water-soluble polymer emulsion.
In the step (1), the mixing time in the mud mixer is 5-15 h.
In the step (2), the process of vacuum mud refining is as follows: putting the obtained mud blank after mixing into mud into a vacuum mud-smelting machine, regulating the vacuum degree to 90kPa, the rotation speed of the mud-smelting machine to 5-20 r/min, and the mud-smelting time to 3-5 h, if the temperature of the mud blank is higher than the ambient temperature by 20 ℃, immediately stopping the mud-smelting machine, and continuously smelting the mud when the temperature is equal to or lower than the room temperature by + -5 ℃; the mud blank ageing process comprises the following steps: the mud blank after vacuum mud refining is wrapped by a plastic film and placed in a dark and cool environment for ageing, the environment humidity is required to be 50-80%, and the ageing time is 12-48 h.
In the step (3), the vacuum extrusion process is as follows: putting the aged mud blank into a vacuum extruder with an inclination angle of 60 degrees for extrusion, wherein the vacuum degree of the extruder is 90kPa; under the extrusion force of 600-900 KN, the mud blank firstly passes through a 120-mesh stainless steel screen to remove particle impurities, and then passes through a metal die with a certain density to obtain the fly ash-based honeycomb ceramic wet blank with the required pore density.
In the step (3), the vacuum extruder can replace metal dies with different hole densities, hole sizes and shapes according to the use requirements, wherein the extruded honeycomb ceramics (round, square and triangular) with different appearances have different flow areas and can be suitable for different fluid flow rate conditions; the cell density and cell size of the honeycomb ceramic have a large impact on its overall mechanical strength and fluid pressure drop.
In the step (4), the water content on the surface of the blank shaped by the microwaves is rapidly reduced, the shape is stable, but the interior of the blank also contains a large amount of water, and the blank is put into an oven for drying treatment, wherein the drying treatment process is as follows: drying in an oven at 60 ℃ for 12 hours, then raising the temperature of the oven to 110 ℃ and continuously drying for 12 hours, wherein the green body is thoroughly dried; and (3) after natural cooling, carrying out end face processing on the dried honeycomb ceramics to obtain a neat honeycomb ceramic end face.
In the step (5), in the high-temperature sintering process, the sintering temperature is 1200 ℃, the heating rate is 5-10 ℃/min, the heat preservation time is 4-6 h, and after the heat preservation time is finished, the material is naturally cooled in a muffle furnace; the pore canal treatment is to use compressed air of 0.5-0.8 MPa to carry out through hole treatment on the honeycomb ceramics so as to remove residual or mixed ceramic particles in the pore canal.
The invention provides a new method for preparing honeycomb ceramics by taking coal-fired fly ash as a raw material, which can meet the requirements of industrial production. The advantages are mainly expressed as follows:
1. the technological process of the method comprises the following steps: ball milling and drying fly ash, preparing a mud blank, vacuum mud refining, ageing the mud blank, vacuum extrusion molding, microwave shaping, drying by a baking oven, high-temperature sintering and processing through holes. The fly ash-based honeycomb ceramic produced by the formula and the process has excellent acid and alkali resistance, high thermal stability and thermal expansion coefficient lower than 1.0 x 10 -6 and/C. The inventionThe ceramic honeycomb has the advantages of good chemical stability, acid and alkali resistance and organic solvent resistance; the rapid-heating and rapid-cooling resistance performance is excellent, and the working temperature can reach more than 1000 ℃; the antibacterial property is good, and the antibacterial agent is not easy to degrade by bacteria; the method has the advantages of strong structural stability, low preparation cost, simple and convenient operation method, no environmental pollution and the like, and provides a feasible high-value resource utilization way for the coal-fired fly ash.
2. The adopted main raw material fly ash has similar chemical composition with common mineral raw materials such as cordierite, kaolin, talcum and the like, and has fine particle size, good stability and simple utilization process;
3. the coal-fired fly ash is produced by high-temperature firing of a coal-fired boiler, has excellent thermal stability, and can obviously reduce the thermal expansion coefficient of honeycomb ceramics;
4. the water-soluble paraffin wax (paraffin wax emulsion) or water-soluble polymer solution is introduced, so that the adhesive can be used as a binder for the mud blank, can be used as a lubricant for reducing the extrusion molding process, can be used as a shaping agent for honeycomb ceramic molding after solidification, and can also be used for preventing cracking in the mud blank drying process.
5. In the vacuum mud refining process, residual air in mud cakes can be removed in a vacuum environment, so that the density and plasticity of mud materials are improved, the mud materials are uniform in structure, the forming performance is improved, and the drying strength and the mechanical strength after forming are improved;
6. in the vacuum extrusion process, a 120-mesh stainless steel screen in the vacuum extruder can effectively filter out particle impurities in the mud blank, and improve the extrusion performance of the mud blank; the vacuum extruder can replace metal dies with different hole densities, hole sizes and shapes according to the use requirements. The extruded honeycomb ceramics (round, square and triangular) with different appearances have different flow areas and can be suitable for different fluid flow rate conditions; the cell density and cell size of the honeycomb ceramic have a large impact on its overall mechanical strength and fluid pressure drop.
7. The microwave shaping adopts a microwave oven for shaping, so that the surface moisture of the wet honeycomb ceramic blank can be rapidly evaporated to form a honeycomb ceramic blank with stable shape, and the mud blank is prevented from collapsing in the subsequent processing step. The high fire treatment is carried out for 5min, which is determined according to a large amount of experimental data analysis, under the working condition, the moisture dryness on the surface of the mud blank is moderate, and meanwhile, the reduction of the integral mechanical strength caused by the rapid volatilization of the internal moisture is avoided;
8. in the process of drying the blank body after microwave shaping, the blank body is firstly dried at a low temperature of 60 ℃ so as to avoid the formation of holes in the blank body or the breakage of the blank body caused by rapid evaporation of water under the condition of overhigh temperature. After drying treatment for 12 hours at 60 ℃, basically removing water, and continuing to dry for 12 hours at 110 ℃, wherein the green body is thoroughly dried; and drying and cooling the blank, and then carrying out end face processing on the blank to obtain a neat end face through the end face processing. Meanwhile, the blank subjected to drying treatment does not have better mechanical strength, so that the processing of the end face and the corners is facilitated;
9. in the high-temperature sintering process, the heating rate is controlled, specifically, the heating rate is 5-10 ℃/min, and after the sintering is completed, the material is naturally cooled in a muffle furnace.
Detailed Description
The present invention is described in detail below with reference to examples.
The invention provides a preparation method of coal ash-based honeycomb ceramics, which takes coal ash as a raw material to prepare the honeycomb ceramics, wherein the coal ash is solid waste formed by high-temperature combustion of coal fuel of a coal-fired power plant, is homogeneous powder, and has the particle size of 1-100 mu m. Compared with the traditional production process which adopts kaolin, talcum, mushroom, chlorite and the like, the use of mineral raw materials can be greatly reduced, and meanwhile, the electric energy loss in the ball milling process can be greatly reduced due to the homogeneous powder structure;
in the fly ash composition used in the examples below, siO 2 The content was 44.27wt.%, of Al 2 O 3 The content is 34.64wt.%, the sum of the contents is 78.91wt.%, and the high-silicon aluminum fly ash is a potential aluminosilicate mineral material. Meanwhile, the fly ash is produced at high temperature in the coal burning process, and the contained silicon and aluminum elements mainly adopt mullite (3 Al 2 O 3 ·2SiO 2 Or 2Al 2 O 3 ·SiO 2 ) In the form of (C) compared with the prior artIn the process, various materials are mixed to prepare the honeycomb ceramic, so that the elements are distributed more uniformly, and the prepared fly ash-based honeycomb ceramic has better thermal stability and mechanical hardness; table 1 shows the physicochemical properties of the fly ash.
Physical and chemical properties of fly ash described in Table 1 examples
SiO 2 Content of 1 Al 2 O 3 Content of 1 SiO 2 +Al 2 O 3 Content of Specific surface area 2 Pore volume 2 Average pore diameter 2
44.27wt.% 34.64wt.% 78.91wt.% 6.55m 2 /g 0.015cm 3 /g 9.7nm
Note that: 1 the content of the fly ash element is determined according to XRF (X-ray fluorescence spectroscopy); 2 the specific surface area, the unit mass pore volume and the average pore diameter of the fly ash are measured according to a nitrogen adsorption and desorption curve;
the specific surface area of the fly ash shown in Table 1 was 6.55m 2 Per gram, pore volume of 0.015cm 3 The average pore diameter of the ceramic is 9.7nm, and the ceramic is a typical porous material, and the honeycomb ceramic prepared by using the ceramic as a raw material has the characteristics of small density and light weight.
Example 1:
the embodiment adopts fly ash as a raw material to synthesize the fly ash-based honeycomb ceramics with triangular pore canals, and the specific process is as follows:
1. the method takes the coal-fired fly ash of the circulating fluidized bed boiler as a raw material, and comprises the following specific processes of: adding 1.2 kg of deionized water per kg of fly ash, adding 0.8wt.% of neutral dispersant JA282 in addition, and performing wet ball milling and mixing by using a roller ball mill, wherein the ball-to-material ratio is 2:1, ball milling time is 10h. And (3) drying the mixture in an oven at 180 ℃ for 24 hours after ball milling and discharging, and sieving the obtained uniform and dried fly ash raw material powder with a 120-mesh screen.
2. According to the weight ratio of the dry fly ash obtained after the pretreatment, weighing a hydroxypropyl methyl cellulose solution accounting for 25wt.% of the dry fly ash, weighing paraffin emulsion accounting for 3wt.% of the dry fly ash, and putting the paraffin emulsion into a mud mixer for mixing to obtain mud, wherein the mixing time is 10 hours. The hydroxypropyl methylcellulose solution is prepared by dissolving hydroxypropyl methylcellulose in water, and has a concentration of 35wt.%.
3. Putting the mixed mud blank into a vacuum mud refining machine, regulating the vacuum degree to 90kPa, refining the mud for 3 hours at the speed of 10r/min, wrapping the mud blank with a plastic film, and placing the plastic film in a dark and cool environment for ageing, wherein the environment humidity is required to be 50-80%, and the ageing time is 24 hours.
4. And (3) putting the aged mud blank into a vacuum extruder for extrusion, wherein the vacuum degree is 90kPa, and under the extrusion force of 800KN, the mud blank firstly passes through a 120-mesh stainless steel screen to remove particle impurities, and then passes through a metal die with 100mm and 600 holes to obtain the fly ash-based honeycomb ceramic wet blank with triangular pore channels.
5. Immediately cutting the wet blank into 50mm blanks by using a stainless steel wire after extrusion, rapidly putting the blanks into a microwave oven for shaping and drying, and selecting high fire and microwave time of 5min for shaping. Then placing the green body into an oven, drying at 60 ℃ for 12 hours, then raising the temperature of the oven to 110 ℃, and continuing drying for 12 hours, wherein the green body is thoroughly dried. And (3) after natural cooling, carrying out end face processing on the dried honeycomb ceramics to obtain a honeycomb ceramic blank with neat end faces.
6. And (3) placing the honeycomb ceramic blank with the neat end face into a muffle furnace for high-temperature sintering, wherein the sintering temperature is 1200 ℃, the heating rate is 5 ℃/min, and the heat preservation time is 5h. And (3) naturally cooling, and then carrying out through hole treatment on the honeycomb ceramics by using compressed air of 0.8MPa, so as to remove residual or mixed ceramic particles in the pore channels. The main performance indexes of the prepared fly ash-based honeycomb ceramics are shown in table 2:
TABLE 2 Main Performance index of the honeycomb ceramics prepared in example 1
Performance index Test conditions Test results
Size (mm) - 100*100*50
Shape of the tunnel - Triangle-shaped
Density of pores (individual/100 cm) 2 ) - 600
Compression strengthDegree (MPa) Axial direction 14
Softening temperature (. Degree. C.) - 1420
Water absorption (%) - 21.1
Apparent Density (g/cm) 3 ) - 0.67
Coefficient of thermal expansion (10 -6 /℃) 20~800℃ 0.86
Example 2:
the embodiment adopts the fly ash as the raw material to synthesize the fly ash-based honeycomb ceramics with square pore canals, and the specific process is as follows:
1. the method takes the coal-fired fly ash of the circulating fluidized bed boiler as a raw material, and comprises the following specific processes of: 1.2 kg of deionized water is added per kg of fly ash, a neutral dispersant JA282 accounting for 0.8wt.% of the weight of the fly ash is additionally added, and the wet ball milling mixing is carried out by using a roller ball mill, wherein the ball-to-material ratio is 2.5:1, ball milling time is 8h. And (3) drying the mixture in an oven at 180 ℃ for 24 hours after ball milling and discharging, and sieving the obtained uniform and dried fly ash raw material powder with a 120-mesh screen.
2. According to the standard of the metering ratio, the dry fly ash obtained after the pretreatment is weighed into a methylcellulose solution accounting for 18wt.% of the dry fly ash, and tung oil accounting for 3wt.% of the dry fly ash is weighed and put into a mud mixer to be mixed into mud, wherein the mixing time is 8 hours. The methylcellulose solution is prepared by dissolving hydroxypropyl methylcellulose in water, and has a concentration of 35wt.%.
3. Putting the mixed mud blank into a vacuum mud refining machine, regulating the vacuum degree to 90kPa, refining the mud for 4 hours at the speed of 12r/min, wrapping the mud blank with a plastic film, and placing the plastic film in a dark and cool environment for ageing, wherein the environment humidity is required to be 50-80%, and the ageing time is 36 hours.
4. And (3) putting the aged mud blank into a vacuum extruder for extrusion, wherein the vacuum degree is 90kPa, and under the extrusion force of 800KN, the mud blank firstly passes through a 120-mesh stainless steel screen to remove particle impurities, and then passes through a metal die with 100mm and 400 holes to obtain the coal ash-based honeycomb ceramic wet blank with round pore channels.
5. Immediately cutting the wet blank into 50mm blanks by using a stainless steel wire after extrusion, rapidly putting the blanks into a microwave oven for shaping and drying, and selecting high fire and microwave time of 5min for shaping. Then placing the green body into an oven, drying at 60 ℃ for 12 hours, then raising the temperature of the oven to 110 ℃, and continuing drying for 12 hours, wherein the green body is thoroughly dried. And (3) after natural cooling, carrying out end face processing on the dried honeycomb ceramics to obtain a honeycomb ceramic blank with neat end faces.
6. And (3) placing the honeycomb ceramic blank with the neat end face into a muffle furnace for high-temperature sintering, wherein the sintering temperature is 1200 ℃, the heating rate is 8 ℃/min, and the heat preservation time is 4 hours. And (3) naturally cooling, and then carrying out through hole treatment on the honeycomb ceramics by using compressed air of 0.6MPa, so as to remove residual or mixed ceramic particles in the pore channels. The main performance indexes of the prepared fly ash-based honeycomb ceramics are shown in table 3:
TABLE 3 Main Performance index of the honeycomb ceramics prepared in example 2
Performance index Test conditions Test results
Size (mm) - 100*100*50
Shape of the tunnel - Round shape
Density of pores (individual/100 cm) 2 ) - 400
Compressive Strength (MPa) Axial direction 13.2
Softening temperature (. Degree. C.) - 1464
Water absorption (%) - 19.6
Apparent Density (g/cm) 3 ) - 0.63
Coefficient of thermal expansion (10 -6 /℃) 20~800℃ 0.88

Claims (10)

1. A preparation method of fly ash-based honeycomb ceramics is characterized in that: the method for preparing the honeycomb ceramics by taking the fly ash as the raw material comprises the following steps:
(1) Preparing a ceramic mud blank: mixing fly ash, binder solution and lubricant in a mud mixer to obtain ceramic mud blank; wherein the weight of the binder solution is 20-35 wt.% of the weight of the fly ash, and the weight of the lubricant is 2-5 wt.% of the weight of the fly ash;
(2) Performing vacuum mud refining and mud blank aging treatment on the ceramic mud blank obtained in the step (1);
(3) Carrying out vacuum extrusion on the mud blank subjected to the ageing treatment in the step (2) to obtain a fly ash-based honeycomb ceramic wet blank with the required pore density;
(4) Immediately cutting the wet blank by using a stainless steel wire to a required length after vacuum extrusion, and rapidly putting the wet blank into a microwave oven for microwave shaping; drying in an oven after microwave shaping, naturally cooling, and processing the end face of the dried honeycomb ceramic to obtain a honeycomb ceramic blank with a neat end face;
(5) And (3) placing the honeycomb ceramic blank with the neat end face obtained after the treatment in the step (4) into a muffle furnace for high-temperature sintering and pore canal treatment, and obtaining the fly ash-based honeycomb ceramic.
2. The method for preparing the fly ash-based honeycomb ceramic according to claim 1, wherein: the fly ash is solid waste formed by high-temperature combustion of coal fuel in a coal-fired power plant, is homogeneous powder, and has a particle size of 1-100 mu m.
3. The method for preparing the fly ash-based honeycomb ceramic according to claim 1, wherein: in the step (1), the raw material fly ash is subjected to pretreatment before use, wherein the pretreatment is ball milling, drying and sieving treatment which are sequentially carried out; the ball milling treatment process comprises the following steps: according to the proportion of adding 1-2 kg of deionized water into each kg of raw material fly ash, adding neutral dispersant JA282 accounting for 0.1-3 wt.% of the weight of the fly ash, and carrying out wet ball milling mixing by using a roller ball mill, wherein the ball-to-material ratio is 1:1 to 3:1, ball milling time is 5-20 h; the drying treatment process comprises the following steps: drying the ball-milled discharge in an oven at 50-200 ℃ for 24-48 h to obtain uniformly mixed and dried fly ash raw material powder; the sieving treatment is to naturally cool the pulverized coal ash powder after ball milling and drying in a baking oven, and then directly pass through a 120-mesh screen, wherein the upper part of the screen is further crushed and then is continuously sieved.
4. The method for preparing the fly ash-based honeycomb ceramic according to claim 1, wherein: in the step (1), the binder solution is prepared by dissolving a binder in water to prepare a binder solution with the concentration of 10-35 wt%, wherein the binder is methyl cellulose, hydroxypropyl methyl cellulose or hydroxyethyl methyl cellulose; the lubricant is vegetable oil, paraffin emulsion or water-soluble polymer emulsion.
5. The method for preparing the fly ash-based honeycomb ceramic according to claim 1, wherein: in the step (1), the mixing time in the mud mixer is 5-15 h.
6. The method for preparing the fly ash-based honeycomb ceramic according to claim 1, wherein: in the step (2), the process of vacuum mud refining is as follows: putting the obtained mud blank after mixing into mud into a vacuum mud-smelting machine, regulating the vacuum degree to 90kPa, the rotation speed of the mud-smelting machine to 5-20 r/min, and the mud-smelting time to 3-5 h, if the temperature of the mud blank is higher than the ambient temperature by 20 ℃, immediately stopping the mud-smelting machine, and continuously smelting the mud when the temperature is equal to or lower than the room temperature by + -5 ℃; the mud blank ageing process comprises the following steps: the mud blank after vacuum mud refining is wrapped by a plastic film and placed in a dark and cool environment for ageing, the environment humidity is required to be 50-80%, and the ageing time is 12-48 h.
7. The method for preparing the fly ash-based honeycomb ceramic according to claim 1, wherein: in the step (3), the vacuum extrusion process is as follows: putting the aged mud blank into a vacuum extruder with an inclination angle of 60 degrees for extrusion, wherein the vacuum degree of the extruder is 90kPa; under the extrusion force of 600-900 KN, the mud blank firstly passes through a 120-mesh stainless steel screen to remove particle impurities, and then passes through a metal die with a certain density to obtain the fly ash-based honeycomb ceramic wet blank with the required pore density.
8. The method for preparing the fly ash-based honeycomb ceramic according to claim 7, wherein: in the step (3), the vacuum extruder can replace metal dies with different hole densities, hole sizes and shapes according to the use requirements, wherein the extruded honeycomb ceramics (round, square and triangular) with different appearances have different flow areas and can be suitable for different fluid flow rate conditions; the cell density and cell size of the honeycomb ceramic have a large impact on its overall mechanical strength and fluid pressure drop.
9. The method for preparing the fly ash-based honeycomb ceramic according to claim 1, wherein: in the step (4), the water content on the surface of the blank shaped by the microwaves is rapidly reduced, the shape is stable, but the interior of the blank also contains a large amount of water, and the blank is put into an oven for drying treatment, wherein the drying treatment process is as follows: drying in an oven at 60 ℃ for 12 hours, then raising the temperature of the oven to 110 ℃ and continuously drying for 12 hours, wherein the green body is thoroughly dried; and (3) after natural cooling, carrying out end face processing on the dried honeycomb ceramics to obtain a neat honeycomb ceramic end face.
10. The method for preparing the fly ash-based honeycomb ceramic according to claim 1, wherein: in the step (5), in the high-temperature sintering process, the sintering temperature is 1200 ℃, the heating rate is 5-10 ℃/min, the heat preservation time is 4-6 h, and after the heat preservation time is finished, the material is naturally cooled in a muffle furnace; the pore canal treatment is to use compressed air of 0.5-0.8 MPa to carry out through hole treatment on the honeycomb ceramics so as to remove residual or mixed ceramic particles in the pore canal.
CN202310671922.4A 2023-06-08 2023-06-08 Preparation method of fly ash-based honeycomb ceramic Pending CN116903386A (en)

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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20100117215A (en) * 2009-04-24 2010-11-03 강릉원주대학교산학협력단 Fabrication of honeycomb type porous cordierite ceramic filter using fly-ash
CN102875128A (en) * 2012-10-30 2013-01-16 华北水利水电学院 Pulverized fuel ash-based heat storage honeycomb ceramic and preparation method thereof
CN106747316A (en) * 2016-11-21 2017-05-31 武汉理工大学 A kind of method that utilization flyash and shale prepare thermo store honeycomb ceramic
CN111018560A (en) * 2019-12-24 2020-04-17 北京大学 Multi-scale pore honeycomb ceramic and preparation method thereof
CN115504803A (en) * 2022-09-14 2022-12-23 浙江天地环保科技股份有限公司 Fly ash based cordierite honeycomb ceramic and preparation method thereof
CN115972401A (en) * 2022-12-16 2023-04-18 浙江天地环保科技股份有限公司 Fly ash based cordierite honeycomb ceramic preparation system

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20100117215A (en) * 2009-04-24 2010-11-03 강릉원주대학교산학협력단 Fabrication of honeycomb type porous cordierite ceramic filter using fly-ash
CN102875128A (en) * 2012-10-30 2013-01-16 华北水利水电学院 Pulverized fuel ash-based heat storage honeycomb ceramic and preparation method thereof
CN106747316A (en) * 2016-11-21 2017-05-31 武汉理工大学 A kind of method that utilization flyash and shale prepare thermo store honeycomb ceramic
CN111018560A (en) * 2019-12-24 2020-04-17 北京大学 Multi-scale pore honeycomb ceramic and preparation method thereof
CN115504803A (en) * 2022-09-14 2022-12-23 浙江天地环保科技股份有限公司 Fly ash based cordierite honeycomb ceramic and preparation method thereof
CN115972401A (en) * 2022-12-16 2023-04-18 浙江天地环保科技股份有限公司 Fly ash based cordierite honeycomb ceramic preparation system

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