CN111960851A - Method for preparing cordierite ceramic filter plate based on aluminum ash raw material - Google Patents

Method for preparing cordierite ceramic filter plate based on aluminum ash raw material Download PDF

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CN111960851A
CN111960851A CN202010900300.0A CN202010900300A CN111960851A CN 111960851 A CN111960851 A CN 111960851A CN 202010900300 A CN202010900300 A CN 202010900300A CN 111960851 A CN111960851 A CN 111960851A
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aluminum ash
filter plate
ceramic filter
cordierite ceramic
aluminum
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CN111960851B (en
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冯晓强
王旭东
牛文军
于长军
乔继才
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Zhengzhou Jingwei Technology Industrial Co ltd
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    • 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
    • C04B38/00Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
    • C04B38/06Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by burning-out added substances by burning natural expanding materials or by sublimating or melting out added substances
    • C04B38/063Preparing or treating the raw materials individually or as batches
    • C04B38/0635Compounding ingredients
    • C04B38/0645Burnable, meltable, sublimable materials
    • C04B38/067Macromolecular compounds
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D39/00Filtering material for liquid or gaseous fluids
    • B01D39/14Other self-supporting filtering material ; Other filtering material
    • B01D39/20Other self-supporting filtering material ; Other filtering material of inorganic material, e.g. asbestos paper, metallic filtering material of non-woven wires
    • B01D39/2068Other inorganic materials, e.g. ceramics
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    • 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
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/16Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on silicates other than clay
    • C04B35/18Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on silicates other than clay rich in aluminium oxide
    • C04B35/195Alkaline earth aluminosilicates, e.g. cordierite or anorthite
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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
    • C04B35/62204Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products using waste materials or refuse
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    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/65Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
    • C04B2235/656Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
    • C04B2235/6562Heating rate
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    • C04B2235/65Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
    • C04B2235/656Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
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    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/65Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
    • C04B2235/66Specific sintering techniques, e.g. centrifugal sintering
    • C04B2235/661Multi-step sintering
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    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
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    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
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    • Y02P10/00Technologies related to metal processing
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  • Filtering Materials (AREA)
  • Compositions Of Oxide Ceramics (AREA)

Abstract

The invention provides a method for preparing a cordierite ceramic filter plate based on an aluminum ash raw material, which mainly takes 30-60% of aluminum ash, 20-55% of talc and 20-50% of quartz sand as main materials, takes a binder (accounting for 1-5% of the weight of the main materials) and an impurity removing agent (accounting for 0.5-5% of the weight of the aluminum ash) as auxiliary materials, and wetly grinds the powder and water according to the weight ratio of 1-4: 1 for pulping; immersing the polyurethane foam board into the slurry to prepare a blank, airing and drying; finally, high-temperature oxygen-enriched sintering is carried out, the porosity of the obtained cordierite ceramic filter plate is more than or equal to 85%, the cordierite phase is more than or equal to 95%, and the thermal shock resistance is more than or equal to 5 times; the resource utilization of the aluminum ash is realized, the natural resources are saved, and the production cost of the ceramic filter plate is reduced.

Description

Method for preparing cordierite ceramic filter plate based on aluminum ash raw material
Technical Field
The invention relates to the technical field of preparation of filter materials, in particular to a method for preparing a cordierite ceramic filter plate based on an aluminum ash raw material.
Background
The aluminum ash is waste generated in the industrial production process of aluminum, mainly comprises simple substance aluminum, aluminum compounds, silicon oxide, magnesium oxide, sodium salt, potassium salt, fluoride salt, titanium oxide and the like, and has toxicity and inflammability. Scum generated on the surface of the melt in the processes of transferring, purifying and impurity removing of the melt in the electrolytic aluminum process, scum (salt slag and aluminum ash) generated on the surface of the melt in the processes of transferring, purifying and impurity removing of the waste aluminum smelting melt, and salt slag and secondary aluminum ash generated in the process of recovering metal aluminum from aluminum ash and aluminum slag by a molten salt method are listed in 2019 edition national hazardous waste records. According to statistics, 15-30 kg of aluminum ash is probably generated every 1 ton of aluminum is produced, the domestic aluminum yield in 2019 is 3500 ten thousand tons, the generated aluminum ash is about 52.5-105 ten thousand tons, and the harmlessness and the recycling of the aluminum ash are problems which are urgently needed to be solved in the aluminum industrial production.
On the other hand, the ceramic has the characteristics of high temperature resistance, corrosion resistance and good thermal shock resistance, the interior of the ceramic filter plate is mostly of a mutually communicated microporous structure, the specific surface area is large, the adsorption capacity is strong, and the ceramic filter plate is widely applied to the fields of filtration dehydration of metal and non-metal concentrates, filtration and impurity removal of metal melts, solid-liquid separation in the environmental protection industry and the like; the current ceramic filter plates have large demand, and the existing sources are difficult to meet the requirements in various production.
Disclosure of Invention
The invention aims to solve the technical problems that the method for preparing the cordierite ceramic filter plate based on the aluminum ash raw material is provided, so that the harmless and resource utilization of the aluminum ash is realized, and the technical problems that the ceramic filter plate consumes a large amount of natural resources, is high in production and has output which is difficult to meet the requirement in the prior art are solved.
In order to solve the technical problems, the invention adopts the following technical scheme:
a method for preparing a cordierite ceramic filter plate based on an aluminum ash raw material is designed, and comprises the following steps:
(1) mixing 30-60% of aluminum ash, 20-55% of talcum powder and 20-50% of quartz sand into a main material in percentage by weight;
(2) adding a binder into the main material according to 1-5% of the weight of the main material, and adding an impurity removing agent into the main material according to 0.5-5% of the weight of the aluminum ash to prepare powder;
(3) mixing the obtained powder with water according to the weight ratio of 1-4: 1, and wet-grinding to obtain slurry;
(4) taking the polyurethane foam board to fully soak the slurry, fishing out, and draining or extruding out the redundant slurry to obtain a sizing board;
(5) drying the sizing plate in the air and drying to obtain a plate blank;
(6) and (3) coking the foam board at low temperature (300-.
The binder is at least one of polyvinyl alcohol, pulp powder, hydroxypropyl methylcellulose and hydroxypropyl methylcellulose sodium.
The impurity removing agent is at least one of ammonium fluoride, ammonium chloride, aluminum fluoride and ammonium carbonate; the impurity removing agent can rapidly and thoroughly remove sodium salt, potassium salt and other impurities in the aluminum ash, and simultaneously promotes aluminum nitride in the aluminum ash to be rapidly oxidized and denitrified to generate nontoxic and harmless nitrogen, thereby ensuring environmental protection and no pollution.
The polyurethane foam board has a density of 10-60 PPI.
In the step (6), the sintering temperature is 1300-,
the temperature raising step during sintering is as follows: the temperature rise rate of 0-300 ℃ stage is 30 ℃/h, the temperature rise rate of 300-550 ℃ stage is 20 ℃/h, the temperature rise rate of 550-1000 ℃ stage is 15 ℃/h, the oxygen content is controlled to be 5-12% (so as to ensure that metal aluminum and aluminum nitride in the aluminum ash are fully oxidized), the temperature rise rate of 1000-sintering final temperature stage is 20 ℃/h, and the aluminum ash is cooled along with the furnace after heat preservation.
In the step (3), the wet grinding particle size of the powder is controlled to be 325-400 meshes.
In the step (5), the sizing plate is naturally aired for 24 hours and dried for 12 hours at the temperature of 150 ℃.
The aluminum ash contains less than or equal to 5 percent of Al, less than or equal to 10 percent of AlN and Al2O3≥80%、SiO2≤0.5%、CaO≤0.5%、MgO≤0.5、Fe2O3Less than or equal to 0.5 percent and the granularity is more than or equal to 100 meshes.
Compared with the prior art, the invention has the main beneficial technical effects that:
1. compared with the ceramic filter plate made of alumina and silicon carbide materials, the ceramic filter plate prepared by the method of the invention has the following advantages: the cordierite ceramic filter plate prepared by the invention has lower thermal expansion coefficient and excellent high-temperature thermal shock resistance, and can be used for a long time in an environment with large cold-hot temperature difference.
2. The invention realizes the harmlessness and reclamation of the aluminum ash, saves natural resources, reduces the production cost (metal aluminum burns, releases a large amount of heat, consumes less fuel in the preparation process, and the price of the aluminum ash raw material is far lower than that of alumina or aluminum oxide).
3. The cordierite ceramic filter plate prepared by the invention fully utilizes the aluminum and magnesium components in the aluminum ash, the porosity of the finished product is more than or equal to 85 percent, the cordierite phase (silicate mineral) is more than or equal to 95 percent, and the thermal shock resistance is more than or equal to 5 times; the finished product has good fire resistance and low thermal expansion rate.
4. In the preparation process, a small amount of HF gas is discharged, the HF gas is in an environment-friendly allowable range and can be effectively recycled, and the finished product does not contain fluoride.
Detailed Description
The following examples are given to illustrate specific embodiments of the present invention, but are not intended to limit the scope of the present invention in any way.
The starting materials referred to in the following examples are, unless otherwise specified, all commercially available conventional starting materials; the assays or detection methods referred to are conventional, unless otherwise specified.
Example 1: method for preparing cordierite ceramic filter plate
37 parts of aluminum ash (containing 5% of Al, 10% of AlN and Al)2O3 70%、SiO2 3%、MgO 1%,TiO22.2 percent of chlorine salt and fluorine salt impurities, 45 parts of talcum (with the purity of 98.5 percent) and 23 parts of quartz sand (with the purity of 99 percent) are uniformly mixed, 3 parts of polyvinyl alcohol binder, 1 part of ammonium fluoride and 0.5 part of ammonium carbonate mixture are added, the powder and water are mixed according to the weight ratio of 4:1, and wet-milled to 325 meshes by using a ceramic ball milling tank to prepare slurry.
Immersing a polyurethane foam board with the density of 30PPI into the slurry; after the slurry is uniformly soaked, taking out the polyurethane foam board, and extruding redundant slurry; and naturally airing the polyurethane foam board blank adhered with the slurry for 24h, and drying at 150 ℃ for 12 h.
Then sintering is carried out at 1380 ℃, and the specific temperature rise curve is as follows: 0-300 ℃, 30 ℃/h, 300-550 ℃, 20 ℃/h, 550-1000 ℃, 5 ℃/h and 8% of oxygen content, 1000-1380 ℃, 20 ℃/h and 1380 ℃ for heat preservation for 4h, and then cooling along with the furnace to obtain the cordierite ceramic filter plate.
The prepared cordierite ceramic filter plate contains 13.5% of MgO and 13.5% of Al through detection2O3 34.3%、SiO250.2 percent, 96.2 percent of cordierite phase, 85 percent of porosity, 28 percent of pore uniformity and 6 times of thermal shock resistance.
Example 2: method for preparing cordierite ceramic filter plate
42 parts of aluminum ash (containing Al 2%, AlN 5% and Al)2O3 70%、SiO2 5%、MgO 10%,TiO22.2 percent of chlorine salt and fluorine salt impurities, 25 parts of talcum (with the purity of 98.5 percent) and 33 parts of quartz sand (with the purity of 99 percent) are uniformly mixed, 3 parts of polyvinyl alcohol binder, 1 part of ammonium fluoride and 0.5 part of ammonium carbonate mixture are added, the powder and water are mixed according to the weight ratio of 1:1, and wet-milled to 400 meshes by using a ceramic ball milling tank to prepare slurry.
Dipping a 20PPI polyurethane foam board into the slurry; after the slurry is uniformly soaked, taking out the polyurethane foam board, and extruding redundant slurry; and naturally airing the polyurethane foam board blank adhered with the slurry for 24h, and drying at 150 ℃ for 12 h.
Then sintering is carried out at 1350 ℃, and the specific temperature rising system is as follows: at 0-300 ℃, 30 ℃/h, 300-.
The prepared cordierite ceramic filter plate contains 13.5% of MgO and 13.5% of Al through detection2O3 34.6%、SiO250 percent, 95.6 percent of cordierite phase, 87.5 percent of porosity, 19 percent of pore uniformity and 7 times of thermal shock resistance.
Example 3: method for preparing cordierite ceramic filter plate
36 parts of aluminum ash (containing 5% of Al, 8% of AlN and Al)2O3 75%、SiO2 1%、MgO 1%,TiO22.5 percent of chlorine salt and fluorine salt impurities, 40 parts of talcum (with the purity of 98.5 percent) and 24 parts of quartz sand (with the purity of 99 percent) are uniformly mixed, 3 parts of polyvinyl alcohol binder, 1 part of ammonium fluoride and 0.5 part of ammonium carbonate mixture are added, the powder and water are mixed according to the weight ratio of 3:2, and wet milling is carried out by a ceramic ball milling tank until the particle size is 350 meshes, thus preparing slurry.
Immersing a polyurethane foam board with the density of 10PPI into the slurry; and after the slurry is uniformly soaked, taking out the polyurethane foam board, and draining redundant slurry.
And naturally airing the polyurethane foam board blank adhered with the slurry for 24h, and drying at 150 ℃ for 12 h.
Then sintering is carried out at 1300 ℃, and the specific temperature rise step is as follows: at 0-300 ℃, 30 ℃/h, 300-550 ℃, 20 ℃/h, 550-1000 ℃, 5 ℃/h and 5 percent of oxygen content, and at 1000-1300 ℃, 20 ℃/h and 1300 ℃ for 6h, and then cooling along with the furnace to obtain the cordierite ceramic filter plate.
The prepared cordierite ceramic filter plate contains 13.2 percent of MgO and 13.2 percent of Al through detection2O3 34%、SiO250 percent, 96.8 percent of cordierite phase, 87.5 percent of porosity, 19 percent of pore uniformity and 5 times of thermal shock resistance.
The present invention is described in detail with reference to the examples above; however, it will be understood by those skilled in the art that various changes in the specific parameters of the embodiments described above may be made or equivalent substitutions of related materials and steps may be made without departing from the spirit of the invention, thereby forming a plurality of specific embodiments, all of which are within the scope of common variations of the invention and will not be described in detail herein.

Claims (9)

1. A method for preparing a cordierite ceramic filter plate based on an aluminum ash raw material is characterized by comprising the following steps:
(1) mixing 30-60% of aluminum ash, 20-55% of talcum powder and 20-50% of quartz sand into a main material in percentage by weight;
(2) then adding a binder into the main material according to 1-5% of the weight of the main material, adding an impurity removing agent into the main material according to 0.5-5% of the weight of the aluminum ash, and mixing the main material and the aluminum ash into powder;
(3) mixing the obtained powder with water according to the weight ratio of 1-4: 1, and wet-grinding to obtain slurry;
(4) taking the polyurethane foam board to fully soak the slurry, fishing out, and draining or extruding out the redundant slurry to obtain a sizing board;
(5) drying the sizing plate in the air and drying to obtain a plate blank;
(6) and (4) coking the foam board at a low temperature and sintering the foam board in a high-temperature oxygen-enriched environment to obtain the cordierite ceramic filter plate.
2. The method of claim 1, wherein the binder is at least one of polyvinyl alcohol, hydroxypropyl methylcellulose, sodium hydroxypropyl methylcellulose, and pulp powder.
3. The method of claim 1, wherein the cleaning agent is at least one of ammonium fluoride, ammonium chloride, aluminum fluoride, and ammonium carbonate.
4. The method of producing a cordierite ceramic filter plate based on an aluminum ash feedstock as set forth in claim 1, wherein the polyurethane foam plate has a density of 10 to 60 PPI.
5. The method for preparing a cordierite ceramic filter plate based on an aluminum ash raw material as set forth in claim 1, wherein the sintering temperature is 1300-1420 ℃ and the holding time is 2-5 hours in the step (6).
6. The method of producing a cordierite ceramic filter plate based on an aluminum ash feedstock as set forth in claim 5, wherein the step of raising the temperature during sintering is: the temperature rise rate is 30 ℃/h at the stage of 0-300 ℃, 20 ℃/h at the stage of 300-550 ℃, the temperature rise rate is 15 ℃/h at the stage of 550-1000 ℃, the oxygen content is controlled to be 5-12%, the temperature rise rate is 20 ℃/h at the stage of 1000 ℃ to the final sintering temperature, and the furnace cooling is carried out after heat preservation.
7. The method for preparing a cordierite ceramic filter plate based on an aluminum ash raw material as set forth in claim 1, wherein in the step (3), the wet grinding particle size of the powder is controlled to 325-400 mesh.
8. The method for manufacturing a cordierite ceramic filter plate based on an aluminum ash raw material according to claim 1, wherein in the step (5), the sizing plate is naturally aired for 24 hours and dried at 150 ℃ for 12 hours.
9. The method of claim 1, wherein the aluminum ash comprises 5% or less Al, 10% or less AlN, and 10% or less Al2O3≥80%、SiO2≤0.5%、CaO≤0.5%、MgO≤0.5、Fe2O3Less than or equal to 0.5 percent and the granularity is more than or equal to 100 meshes.
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Cited By (1)

* Cited by examiner, † Cited by third party
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CN116023126A (en) * 2023-02-17 2023-04-28 山东奥福环保科技股份有限公司 High-porosity and large-aperture honeycomb ceramic carrier and preparation method thereof

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GB208716A (en) * 1922-12-21 1925-04-20 Aluminum Co Of America Improvements in or relating to the production of aluminium
JP2004203724A (en) * 2002-10-30 2004-07-22 Kyocera Corp Cordierite porous sintered compact, and ceramic filter obtained by using the same
PT103532A (en) * 2006-07-20 2007-02-28 Inst Superior Tecnico PRODUCTION OF CERAMIC FOAMS OF CORDIERITE BY IN-SITU POLYMERIZATION
US20110143012A1 (en) * 2009-12-11 2011-06-16 Rettenmaier Albert C Methods of algae harvesting utilizing a filtering substance and uses therefor
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