CN115504803A - Fly ash based cordierite honeycomb ceramic and preparation method thereof - Google Patents
Fly ash based cordierite honeycomb ceramic and preparation method thereof Download PDFInfo
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- CN115504803A CN115504803A CN202211119278.1A CN202211119278A CN115504803A CN 115504803 A CN115504803 A CN 115504803A CN 202211119278 A CN202211119278 A CN 202211119278A CN 115504803 A CN115504803 A CN 115504803A
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- fly ash
- honeycomb ceramic
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- 239000010881 fly ash Substances 0.000 title claims abstract description 47
- 239000000919 ceramic Substances 0.000 title claims abstract description 31
- 229910052878 cordierite Inorganic materials 0.000 title claims abstract description 26
- JSKIRARMQDRGJZ-UHFFFAOYSA-N dimagnesium dioxido-bis[(1-oxido-3-oxo-2,4,6,8,9-pentaoxa-1,3-disila-5,7-dialuminabicyclo[3.3.1]nonan-7-yl)oxy]silane Chemical compound [Mg++].[Mg++].[O-][Si]([O-])(O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2)O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2 JSKIRARMQDRGJZ-UHFFFAOYSA-N 0.000 title claims abstract description 26
- 238000002360 preparation method Methods 0.000 title abstract description 6
- 239000000843 powder Substances 0.000 claims abstract description 13
- 239000011230 binding agent Substances 0.000 claims abstract description 11
- 239000002270 dispersing agent Substances 0.000 claims abstract description 10
- 229910052761 rare earth metal Inorganic materials 0.000 claims abstract description 9
- 238000005245 sintering Methods 0.000 claims abstract description 9
- 239000000654 additive Substances 0.000 claims abstract description 8
- 230000000996 additive effect Effects 0.000 claims abstract description 8
- 238000002156 mixing Methods 0.000 claims abstract description 8
- BYMUNNMMXKDFEZ-UHFFFAOYSA-K trifluorolanthanum Chemical compound F[La](F)F BYMUNNMMXKDFEZ-UHFFFAOYSA-K 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 9
- 239000004014 plasticizer Substances 0.000 claims description 9
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 8
- 239000000463 material Substances 0.000 claims description 8
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 6
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 6
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 6
- DOIRQSBPFJWKBE-UHFFFAOYSA-N dibutyl phthalate Chemical compound CCCCOC(=O)C1=CC=CC=C1C(=O)OCCCC DOIRQSBPFJWKBE-UHFFFAOYSA-N 0.000 claims description 6
- 239000004615 ingredient Substances 0.000 claims description 6
- 150000002910 rare earth metals Chemical class 0.000 claims description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 5
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 5
- 239000000454 talc Substances 0.000 claims description 5
- 229910052623 talc Inorganic materials 0.000 claims description 5
- 235000012222 talc Nutrition 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 4
- 150000003839 salts Chemical class 0.000 claims description 4
- 230000032683 aging Effects 0.000 claims description 3
- 238000000498 ball milling Methods 0.000 claims description 3
- 239000000377 silicon dioxide Substances 0.000 claims description 3
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 claims description 2
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims description 2
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims description 2
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- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 2
- 239000005642 Oleic acid Substances 0.000 claims description 2
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims description 2
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- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims description 2
- QCCDYNYSHILRDG-UHFFFAOYSA-K cerium(3+);trifluoride Chemical compound [F-].[F-].[F-].[Ce+3] QCCDYNYSHILRDG-UHFFFAOYSA-K 0.000 claims description 2
- 235000019425 dextrin Nutrition 0.000 claims description 2
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 claims description 2
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 claims description 2
- 229920003063 hydroxymethyl cellulose Polymers 0.000 claims description 2
- 229940031574 hydroxymethyl cellulose Drugs 0.000 claims description 2
- 239000001863 hydroxypropyl cellulose Substances 0.000 claims description 2
- 235000010977 hydroxypropyl cellulose Nutrition 0.000 claims description 2
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims description 2
- 238000004898 kneading Methods 0.000 claims description 2
- 229920000609 methyl cellulose Polymers 0.000 claims description 2
- 239000001923 methylcellulose Substances 0.000 claims description 2
- 235000010981 methylcellulose Nutrition 0.000 claims description 2
- 239000011812 mixed powder Substances 0.000 claims description 2
- 230000007935 neutral effect Effects 0.000 claims description 2
- 229910017604 nitric acid Inorganic materials 0.000 claims description 2
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims description 2
- 235000006408 oxalic acid Nutrition 0.000 claims description 2
- 239000012188 paraffin wax Substances 0.000 claims description 2
- 239000004584 polyacrylic acid Substances 0.000 claims description 2
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 2
- 238000004321 preservation Methods 0.000 claims description 2
- 229910052814 silicon oxide Inorganic materials 0.000 claims description 2
- 229920002545 silicone oil Polymers 0.000 claims description 2
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 claims description 2
- 239000008107 starch Substances 0.000 claims description 2
- 235000019698 starch Nutrition 0.000 claims description 2
- HPNURIVGONRLQI-UHFFFAOYSA-K trifluoroeuropium Chemical compound F[Eu](F)F HPNURIVGONRLQI-UHFFFAOYSA-K 0.000 claims description 2
- 238000005406 washing Methods 0.000 claims description 2
- 229940105963 yttrium fluoride Drugs 0.000 claims description 2
- RBORBHYCVONNJH-UHFFFAOYSA-K yttrium(iii) fluoride Chemical compound F[Y](F)F RBORBHYCVONNJH-UHFFFAOYSA-K 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 1
- 230000000694 effects Effects 0.000 abstract description 4
- -1 rare earth fluoride Chemical class 0.000 abstract description 4
- 238000001125 extrusion Methods 0.000 abstract description 3
- 239000012752 auxiliary agent Substances 0.000 abstract description 2
- 230000009286 beneficial effect Effects 0.000 abstract description 2
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- 239000003245 coal Substances 0.000 description 4
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- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 239000012071 phase Substances 0.000 description 3
- IRPGOXJVTQTAAN-UHFFFAOYSA-N 2,2,3,3,3-pentafluoropropanal Chemical compound FC(F)(F)C(F)(F)C=O IRPGOXJVTQTAAN-UHFFFAOYSA-N 0.000 description 2
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 2
- KLZUFWVZNOTSEM-UHFFFAOYSA-K Aluminum fluoride Inorganic materials F[Al](F)F KLZUFWVZNOTSEM-UHFFFAOYSA-K 0.000 description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- 235000015895 biscuits Nutrition 0.000 description 2
- 238000002485 combustion reaction Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
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- 238000000465 moulding Methods 0.000 description 2
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- 239000002689 soil Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- 229910010413 TiO 2 Inorganic materials 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000004566 building material Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
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- C04B38/0006—Honeycomb structures
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- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
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Abstract
The invention relates to a fly ash based cordierite honeycomb ceramic and a preparation method thereof. The invention has the beneficial effects that: the invention has high fly ash mixing amount, low additive introduction amount and low sintering temperature, thereby having lower cost; in addition, the added binder dispersant and the like remarkably improve the dispersibility of the pug through the effects of steric hindrance and the like on all components in the powder, so that the pug has excellent and stable plasticity and water retention, high solid content, easy extrusion and high yield; and the rare earth fluoride auxiliary agent is added, so that the thermal and mechanical properties of the ceramic are excellent.
Description
Technical Field
The invention relates to the field of high-valued application of coal-based solid wastes and preparation of ceramic heat accumulators, in particular to fly ash-based cordierite honeycomb ceramic and a preparation method thereof.
Background
At present, electric energy mainly comes from thermal power generation, coal for combustion of thermal power generation is mostly pulverized coal after mechanical crushing, and the pulverized coal can generate certain fly ash after sufficient combustion. Although the resource utilization of the fly ash has been advanced in recent years, most of the fly ash still can be only accumulated around a power plant, and a large amount of land resources are occupied. In addition, the waste fly ash causes problems of dust pollution, water pollution, soil pollution and the like.
The main chemical component of the fly ash is SiO 2 、Al 2 O 3 And Fe 2 O 3 About 70% of the total amount, and about 30% of other components such as CaO, mgO, and trace elements. Obviously, the fly ash is a secondary resource and has rich application potential. At present, the fly ash is often used as a building raw material, for soil improvement, for pit/mine backfilling and the like, and the comprehensive utilization technology and level are low. Meanwhile, as the building material market is gradually saturated, the agricultural soil standard is improved, the pit backfilling is seriously influenced by regional factors, and the comprehensive utilization rate of the fly ash is always low. The development of novel structural functional materials with high added values by utilizing the fly ash is an important way and a research hotspot for realizing the high-value utilization of the fly ash.
The molecular formula of cordierite is 2 MgO.2A 1 2 O 3 ·5SiO 2 It is an important ceramic material and has the advantages of large specific heat capacity, low thermal expansion coefficient, good thermal shock resistance and the like. Cordierite is widely used as a heat accumulator material, high-temperature structural ceramic, a catalyst carrier, biological ceramic and the like. Fly ash due to contentHas rich Al and Si resources and can be used for synthesizing cordierite. However, fly ash contains a plurality of impurities, and the impurity ions can replace Mg in cordierite on one hand 2+ Or Al 3+ Ions inhibit the formation of cordierite phase, and on the other hand, excessive glass phase is generated in the high-temperature sintering process, thereby reducing the thermal and mechanical properties of the material. In addition, fly ash, a poor material, has poor moldability, and thus it is difficult to obtain a high-quality ceramic biscuit by extrusion.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provides fly ash-based cordierite honeycomb ceramic and a preparation method thereof.
The first aspect provides a fly ash-based cordierite honeycomb ceramic which is prepared by adding a binder, a plasticizer, a dispersant and water into fly ash and other inorganic ingredient powder; the fly ash is pretreated, and the other inorganic ingredient powder comprises talc, alumina, silica and a rare earth additive; the total mass content of the fly ash and other inorganic auxiliary powder is 100 percent, wherein the pretreated fly ash accounts for 20 to 70 percent, the talcum accounts for 10 to 40 percent, the alumina accounts for 5 to 20 percent, the silicon oxide accounts for 0 to 30 percent, and the rare earth additive accounts for 0.2 to 3.0 percent; the addition amounts of the binder, the plasticizer, the dispersant and the water are respectively 2-10%, 3-10%, 0.1-3% and 13-30% of the total mass of the fly ash and other inorganic ingredient powder.
Preferably, the rare earth auxiliary agent is one or more of lanthanum fluoride, cerium fluoride, europium fluoride and yttrium fluoride; the binder is one or more of starch, dextrin, methylcellulose, hydroxypropyl cellulose, hydroxymethyl cellulose and paraffin; the plasticizer is one or more of glycerol, dibutyl phthalate and oxalic acid; the dispersing agent is one or more of oleic acid, dimethyl silicone oil, polyvinyl alcohol, polyacrylic acid and salts thereof, citric acid and salts thereof, sodium dodecyl benzene sulfonate, triethanolamine and ethylene glycol.
In a second aspect, there is provided a method for preparing the fly ash-based cordierite honeycomb ceramic according to the first aspect, comprising:
s1, treating the fly ash in a 1-30wt% hydrochloric acid or nitric acid solution for 0.5-3h, washing with water to be neutral, and drying;
s2, mixing the pretreated fly ash and other inorganic auxiliary material powder in proportion, and performing dry ball milling;
s3, mixing the mixed powder in the S2 in a powerful mixer, adding a binder, a plasticizer, a dispersant and water, and kneading;
s4, after aging and pugging, continuously extruding and molding the kneaded material under 8-25MPa, wherein the vacuum degree is 0.09-0.1MPa;
s5, drying the obtained honeycomb ceramic green body at 40-120 ℃, and sintering at 1200-1450 ℃, wherein the heating rate is 1-5 ℃/min, and the heat preservation time is 1-4h.
The invention has the beneficial effects that:
(1) Low raw material cost, stable process and high yield. The fly ash is high in mixing amount, the additive is low in introduction amount, and the sintering temperature is low, so that the cost is low; in addition, the added binder dispersant and the like remarkably improve the dispersibility of the pug through the effects of steric hindrance and the like on all components in the powder, so that the pug has excellent and stable plasticity and water-retaining property, high solid content, easy extrusion and high yield.
(2) The ceramic has excellent thermal and mechanical properties. The rare earth fluoride additive added in the invention can promote the stepped phase transition of the fly ash in the process of generating cordierite due to the special lattice distortion generated by rare earth ions; in addition, partial decomposition products can react with specific elements in other raw materials to generate a high-temperature liquid phase so as to promote mass transfer and sintering. The combined action of the mechanisms can obviously improve the density of the material, improve the compressive strength and reduce the thermal expansion coefficient.
Drawings
FIG. 1 is a flow chart of a method for preparing a fly ash-based cordierite honeycomb ceramic.
Detailed Description
The present invention will be further described with reference to the following examples. The following examples are set forth merely to aid in the understanding of the invention. It should be noted that, for a person skilled in the art, several modifications can be made to the invention without departing from the principle of the invention, and these modifications and modifications also fall within the protection scope of the claims of the present invention.
The embodiment of the invention adopts fly ash of a certain domestic coal-fired power plant. The chemical composition of the fly ash is as follows: siO 2 2 :48.77%、 Al 2 O 3 :31.56%、Fe 2 O 3 :5.57%、CaO:5.98%、TiO 2 :1.64%、MgO:0.75%、SO 3 :0.19%。
Example 1
Weighing 12kg of fly ash, adding 2mol/L HCl solution 40L, stirring at 80 ℃ for reaction for 2h, cleaning and drying. Mixing the treated fly ash with talc, alumina, silica and lanthanum fluoride according to a ratio of 50: 0.5, preparing 20kg of powder in total, adding zirconia balls according to the ball-to-ball ratio of 3:1, mixing and ball-milling for 1h. 1kg of binder (hydroxypropyl methylcellulose), 0.6kg of plasticizer (dibutyl phthalate), 0.04kg of citric acid and 4kg of water were added to the above mixture, and mixed vigorously for 30min.
And (3) ageing the pug overnight, extruding by using a vacuum pug mill, continuously extruding and molding under the vacuum degree of 0.095MPa by using a square-hole honeycomb ceramic die under the vacuum degree of 20MPa, and cutting by using a molybdenum wire to obtain a honeycomb ceramic biscuit.
The formed embryo is placed at room temperature overnight and then dried in an oven at 60 ℃ and 110 ℃ for 2h to remove the residual water.
And (3) placing the dried green body in a muffle furnace, heating to 60 ℃ at the speed of 2 ℃/min under the air atmosphere, preserving heat for 2h, heating to 1300 ℃ at the speed of 2 ℃/min, preserving heat for 2h, and sintering to obtain the cordierite honeycomb ceramic.
The test shows that the volume density of the cordierite ceramic is 2.05g/cm 3 The average thermal expansion coefficient at RT-800 ℃ is 2.36 multiplied by 10 -6 /° c, the overall performance is good.
Example 2
The process of example 1 was repeated with lanthanum fluoride incorporation increased to 1.0 wt.%.
The cordierite ceramic of the present invention was tested to have a bulk density of 2.23g/cm 3 。
Example 3
The process of example 1 was repeated with lanthanum fluoride incorporation increased to 1.5 wt.%.
The volume density of the cordierite ceramic is 2.26g/cm 3 . Comparing comparative examples 1 to 3, it can be seen that the degree of densification of cordierite ceramics gradually increases with the increase in the amount of lanthanum fluoride added.
Comparative example 1
Lanthanum fluoride incorporation was reduced to 0wt.% and the process of example 1 was repeated.
The volume density of the cordierite ceramic is 2.01g/cm 3 Coefficient of thermal expansion of 2.98X 10 -6 V. C. The bulk densities of examples 1-3 were all improved over comparative example 1, and the average coefficient of thermal expansion of example 1 was increased by 20.81% over comparative example 1 at RT-800 deg.C, indicating that the addition of lanthanum fluoride promotes sintering and reduces the average coefficient of thermal expansion.
Comparative example 2
The process of example 1 was repeated by replacing the lanthanum fluoride with aluminum fluoride.
The test shows that the volume density of the cordierite ceramic is 2.02g/cm 3 Coefficient of thermal expansion of 2.89X 10 -6 V. C. The bulk density of comparative example 2 is higher than comparative example 1, but lower than example 1. The coefficient of thermal expansion of comparative example 2 is also between that of comparative example and example 1. This shows that the addition of aluminum fluoride has an effect on promoting sintering and improving thermal properties, but at the same addition level, the effect is less than that of lanthanum fluoride.
In conclusion, the invention provides a method for preparing a high-quality cordierite honeycomb ceramic heat accumulator by continuously extruding fly ash, and the method has the advantages of simple process, low raw material cost, good process repeatability and excellent thermal and mechanical properties of the prepared cordierite honeycomb ceramic.
Claims (3)
1. A fly ash based cordierite honeycomb ceramic is characterized in that the honeycomb ceramic is prepared by fly ash and other inorganic ingredient powder with addition of binder, plasticizer, dispersant and water; the fly ash is pretreated, and the other inorganic ingredient powder comprises talc, alumina, silica and a rare earth additive; the total mass content of the fly ash and other inorganic auxiliary powder is 100 percent, wherein the pretreated fly ash accounts for 20 to 70 percent, the talcum accounts for 10 to 40 percent, the alumina accounts for 5 to 20 percent, the silicon oxide accounts for 0 to 30 percent, and the rare earth additive accounts for 0.2 to 3.0 percent; the addition amounts of the binder, the plasticizer, the dispersant and the water are respectively 2-10%, 3-10%, 0.1-3% and 13-30% of the total mass of the fly ash and other inorganic ingredient powder.
2. The fly ash-based cordierite honeycomb ceramic of claim 1, wherein the rare earth additive is one or more of lanthanum fluoride, cerium fluoride, europium fluoride and yttrium fluoride; the binder is one or more of starch, dextrin, methylcellulose, hydroxypropyl cellulose, hydroxymethyl cellulose and paraffin; the plasticizer is one or more of glycerol, dibutyl phthalate and oxalic acid; the dispersing agent is one or more of oleic acid, dimethyl silicone oil, polyvinyl alcohol, polyacrylic acid and salts thereof, citric acid and salts thereof, sodium dodecyl benzene sulfonate, triethanolamine and ethylene glycol.
3. A method for producing the fly ash-based cordierite honeycomb ceramic according to claim 1, comprising:
s1, treating the fly ash in a 1-30wt% hydrochloric acid or nitric acid solution for 0.5-3h, washing with water until the fly ash is neutral, and drying;
s2, mixing the pretreated fly ash and other inorganic auxiliary material powder in proportion, and performing dry ball milling;
s3, mixing the mixed powder in the S2 in an intensive mixer, adding a binder, a plasticizer, a dispersant and water, and kneading;
s4, continuously extruding and forming the kneaded material under the pressure of 8-25MPa after ageing and pugging, wherein the vacuum degree is 0.09-0.1MPa;
s5, drying the obtained honeycomb ceramic green body at 40-120 ℃, and sintering at 1200-1450 ℃, wherein the heating rate is 1-5 ℃/min, and the heat preservation time is 1-4h.
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