CN116425564B - Alumina refractory material and preparation method thereof - Google Patents
Alumina refractory material and preparation method thereof Download PDFInfo
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- CN116425564B CN116425564B CN202310403201.5A CN202310403201A CN116425564B CN 116425564 B CN116425564 B CN 116425564B CN 202310403201 A CN202310403201 A CN 202310403201A CN 116425564 B CN116425564 B CN 116425564B
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- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 title claims abstract description 109
- 239000011819 refractory material Substances 0.000 title claims abstract description 40
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 239000000843 powder Substances 0.000 claims abstract description 126
- 239000011230 binding agent Substances 0.000 claims abstract description 37
- 239000002002 slurry Substances 0.000 claims description 86
- 239000006260 foam Substances 0.000 claims description 48
- 238000003756 stirring Methods 0.000 claims description 47
- 239000002994 raw material Substances 0.000 claims description 27
- 238000005245 sintering Methods 0.000 claims description 23
- 239000002245 particle Substances 0.000 claims description 19
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 18
- 239000007864 aqueous solution Substances 0.000 claims description 14
- 238000000465 moulding Methods 0.000 claims description 10
- DIZPMCHEQGEION-UHFFFAOYSA-H aluminium sulfate (anhydrous) Chemical compound [Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O DIZPMCHEQGEION-UHFFFAOYSA-H 0.000 claims description 9
- 238000000034 method Methods 0.000 claims description 9
- 239000011148 porous material Substances 0.000 claims description 9
- 239000000377 silicon dioxide Substances 0.000 claims description 9
- 238000000227 grinding Methods 0.000 claims description 8
- 229920002134 Carboxymethyl cellulose Polymers 0.000 claims description 7
- 235000010948 carboxy methyl cellulose Nutrition 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 7
- 239000004094 surface-active agent Substances 0.000 claims description 7
- 239000001768 carboxy methyl cellulose Substances 0.000 claims description 3
- 239000008112 carboxymethyl-cellulose Substances 0.000 claims description 3
- RGPUVZXXZFNFBF-UHFFFAOYSA-K diphosphonooxyalumanyl dihydrogen phosphate Chemical compound [Al+3].OP(O)([O-])=O.OP(O)([O-])=O.OP(O)([O-])=O RGPUVZXXZFNFBF-UHFFFAOYSA-K 0.000 claims description 3
- 238000000889 atomisation Methods 0.000 claims description 2
- 239000003822 epoxy resin Substances 0.000 claims description 2
- 229920000647 polyepoxide Polymers 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 1
- 230000000052 comparative effect Effects 0.000 description 16
- 239000000203 mixture Substances 0.000 description 15
- 238000001035 drying Methods 0.000 description 7
- 230000006835 compression Effects 0.000 description 6
- 238000007906 compression Methods 0.000 description 6
- 239000000243 solution Substances 0.000 description 4
- 239000000463 material Substances 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 238000004321 preservation Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 238000000137 annealing Methods 0.000 description 1
- 239000011449 brick Substances 0.000 description 1
- 239000004566 building material Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000000875 high-speed ball milling Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 238000003801 milling Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 238000010791 quenching Methods 0.000 description 1
- 230000000171 quenching effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000000518 rheometry Methods 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
- C04B38/10—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by using foaming agents or by using mechanical means, e.g. adding preformed foam
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/10—Shaped 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 aluminium oxide
- C04B35/101—Refractories from grain sized mixtures
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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- C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
- C04B38/08—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by adding porous substances
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/74—Physical characteristics
- C04B2235/77—Density
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
- C04B2235/9607—Thermal properties, e.g. thermal expansion coefficient
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Abstract
The invention provides an alumina refractory material and a preparation method thereof, wherein the alumina refractory material comprises the following components in percentage by weight: 40-50% of 0.2-1mm alumina hollow spheres, 40-50% of micron-sized spherical hollow powder, 5-15% of alumina powder and 1.5-10% of binding agent; wherein, the micron-sized spherical hollow powder is internally provided with a plurality of closed small cavities, and the overall porosity is 30-60%. According to the invention, the micron-sized spherical hollow powder with a specific structure is introduced into the alumina refractory material and is reasonably compounded with the alumina hollow spheres, the alumina powder and the binding agent, so that the volume density and the heat conductivity coefficient of the alumina refractory material are effectively reduced on the basis of ensuring the strength, the energy is saved, and the cost is reduced.
Description
Technical Field
The invention relates to the field of refractory materials, in particular to an alumina refractory material and a preparation method thereof.
Background
The alumina refractory material is a heat-insulating refractory material which is widely used, and has the advantages of high alumina content, high strength, high use temperature, good thermal shock resistance and the like, so that the alumina refractory material is widely applied to high-temperature kilns in petrochemical industry, and can be used as a heat-insulating material and a high-temperature working lining material.
However, one of the raw materials adopted by the common alumina refractory material is alumina micropowder, has high volume density and high heat conductivity coefficient, directly causes energy waste in the application process, increases the cost and greatly prevents the wide application of the alumina refractory material.
Even if a refractory material using alumina hollow spheres and alumina powder as raw materials has appeared later, it is difficult to combine low thermal conductivity with high strength. That is, there is still a need to develop alumina refractories with good overall properties.
Disclosure of Invention
Aiming at the defects existing in the prior art, the invention provides an alumina refractory material and a preparation method thereof.
In a first aspect, the present invention provides an alumina refractory comprising the following components in weight percent: 40-50% of 0.2-1mm alumina hollow spheres, 40-50% of micron-sized spherical hollow powder, 5-15% of alumina powder and 1.5-10% of binding agent;
wherein, the micron-sized spherical hollow powder is internally provided with a plurality of closed small cavities, and the overall porosity is 30-60%.
According to the invention, the research shows that the micron-sized spherical hollow powder with a certain proportion of closed small cavities and overall porosity within the range of 30-60% is added into the existing refractory material taking the alumina hollow spheres and the alumina powder as raw materials, so that the volume density and the heat conductivity coefficient of the alumina refractory material can be effectively reduced on the basis of ensuring the strength, the energy is saved, and the cost is reduced.
In some embodiments of the invention, the micron-sized spherical hollow powder has a particle size of 50-150 μm, a surface pore size of 2-5 μm, and the small cavities have an average diameter of 5-20 μm.
In some embodiments of the invention, the small cavities have an average wall thickness of 2-5 μm.
In some embodiments of the present invention, the raw material of the micron-sized spherical hollow powder includes 80% or more of alumina by mass fraction.
In some preferred embodiments of the present invention, the raw material of the micron-sized spherical hollow powder is composed of 90-95% by mass of alumina and 5-10% by mass of silica.
In some embodiments of the invention, the micron-scaleThe bulk density of the spherical hollow powder is 0.5-0.8g/cm 3 The heat conductivity coefficient is 0.1-0.2W/(mK).
In some embodiments of the invention, the 0.2-1mm alumina hollow spheres have a bulk density of 0.7-0.9g/cm 3 。
In some embodiments of the invention, the alumina powder has a particle size of less than 50 μm.
In some embodiments of the invention, the binding agent is one or more of aluminum sulfate, aluminum dihydrogen phosphate, epoxy resin, carboxymethyl cellulose.
In a preferred embodiment of the present invention, the micron-sized spherical hollow powder is prepared from 95% by mass of alumina and 5% by mass of silica, and has a particle diameter (D50) of 100 μm, an average diameter of small cavities of 15 μm, an average wall thickness of 3 μm, a surface pore size of 4 μm, and an overall porosity of 50%.
In a second aspect, the present invention provides a method of preparing the alumina refractory described above.
The preparation method provided by the invention comprises the following steps: the components are mixed, formed, dried and sintered, wherein the sintering temperature is 1600-1700 ℃.
In some embodiments of the invention, the binding agent is mixed with water to form an aqueous solution having a concentration of 1.5-10% and then mixed with the remaining components.
In some embodiments of the present invention, the method for preparing an alumina refractory material specifically includes the steps of:
step one, preparing a binding agent and water into an aqueous solution with the concentration of 1.5-10% for later use;
step two, adding 40-50% of 0.2-1mm alumina hollow spheres, 40-50% of micron-sized spherical hollow powder and 5-15% of alumina powder into a mixer for uniform stirring;
step three, stirring for 3-6 hours, and then adding the aqueous solution of the binding agent prepared in the step one into a mixer to continuously stir for 1-3 hours;
step four, placing the prepared mixture into a mould for compression vibration molding, and placing the molded green body into an oven for drying for 24-36h;
and fifthly, placing the dried green body into a muffle furnace for sintering to obtain a product, wherein the sintering temperature is 1600-1700 ℃.
In some embodiments of the present invention, the method for preparing the micron-sized spherical hollow powder includes:
s1: preparing slurry from the powder raw materials and water, and grinding to obtain powder with particle size of 1-10 μm.
Further, the mass fraction of the powder raw material in the slurry is 25-65%.
Preferably, the milling is carried out in a mill at a speed of 50-1000rpm for 12-36 hours.
The grinding rate and time of the slurry influence the granularity of powder in the slurry, the smaller the granularity is, the smaller the charge resistance is, the more easily the charge resistance is accumulated on the surface of foam, the wall thickness of the final spherical hollow powder is influenced, and the surface energy of inorganic powder particles in the process of small thinning can be greatly increased by high-speed ball milling, so that the rheological property of the slurry is influenced.
S2: dividing the ground slurry in the step S1 into two parts of slurry A and slurry B, adding a first binder and a first surfactant into the slurry A, and uniformly stirring to obtain foam slurry C with the diameter of 0.05-0.3mm; and adding a second binder and a second surfactant into the slurry B, and uniformly stirring to obtain foam slurry D with the diameter of 5-50 mu m.
Further, the mass fraction of the first binder is 0.1-3%, and the mass fraction of the first surfactant is 0.1-2%; the mass fraction of the second binder is 0.5-3%, and the mass fraction of the second surfactant is 0.5-2%.
Further, the mass ratio of the slurry A to the slurry B is 1:8-15.
S3: and (3) mixing and uniformly stirring the foam slurry C and the foam slurry D obtained in the step S2.
Further, the stirring time is 20-60min; the stirring rate was 100-900rpm.
Two kinds of foam slurry with different foam sizes are prepared respectively through the step S2, and different binders and surfactants are added respectively, so that the foam with large diameter has small surface energy and the foam with small diameter has large surface energy. In step S3, the two foams are mixed together, and the small foam having a large surface energy is made to enter the inside of the large foam having a small surface energy by stirring.
S4: and (3) carrying out atomization molding on the product obtained in the step (S3) in a molding tower to obtain a spherical hollow powder blank.
Further, an atomizing disc is arranged in the forming tower, and the rotating speed of the atomizing disc is 6000-12000rpm. The rotational speed of the atomizing disk in combination with the slurry rheology in steps S1 and S2 affects the particle size of the final powder.
Further, the inlet temperature of the forming tower is 300-450 ℃; the outlet temperature of the forming tower is not lower than 90 ℃. The inlet and outlet temperature of the forming tower influences the water content and the drying efficiency of the spherical hollow powder blank.
And S5, sintering the spherical hollow powder blank obtained in the step S4, and cooling to obtain the spherical hollow powder.
Further, the sintering temperature is 1400-1500 ℃.
In a third aspect, the present invention provides a refractory article comprising the alumina refractory material described above. Such refractory products include, but are not limited to, refractory bricks, castable, spray coatings, castable, and the like. The refractory product can be used for small heat treatment furnaces such as quenching furnaces, annealing furnaces, box-type electric furnaces, well-type electric furnaces and the like, can also be used for hot blast stoves of tunnel kilns, roller kilns and blast furnaces and other large-scale kilns, and can be widely applied to thermal equipment in industrial departments such as metallurgy, petrochemical industry, machinery, electric power, building materials, aerospace, shipbuilding and the like.
The invention provides an alumina refractory material and a preparation method thereof, which are characterized in that micron-sized spherical hollow powder with a specific structure is introduced into the alumina refractory material and reasonably compounded with alumina hollow spheres, alumina powder and a binding agent, so that the volume density and the heat conductivity coefficient of the alumina refractory material are effectively reduced on the basis of ensuring the strength, the energy is saved, and the cost is reduced.
Drawings
Fig. 1 is a scanning electron microscope image of a micron-sized spherical hollow powder according to example 1 of the present invention.
Detailed Description
Term interpretation:
"prepared from … …" is synonymous with "comprising". The terms "comprising," "including," "having," "containing," or any other variation thereof, as used herein, are intended to cover a non-exclusive inclusion. For example, a composition, step, method, article, or apparatus that comprises a list of elements is not necessarily limited to only those elements but may include other elements not expressly listed or inherent to such composition, step, method, article, or apparatus.
The conjunction "consisting of … …" excludes any unspecified element, step or component. If used in a claim, such phrase will cause the claim to be closed, such that it does not include materials other than those described, except for conventional impurities associated therewith. When the phrase "consisting of … …" appears in a clause of the claim body, rather than immediately following the subject, it is limited to only the elements described in that clause; other elements are not excluded from the stated claims as a whole.
When an equivalent, concentration, or other value or parameter is expressed as a range, preferred range, or a range bounded by a list of upper preferable values and lower preferable values, this is to be understood as specifically disclosing all ranges formed from any pair of any upper range limit or preferred value and any lower range limit or preferred value, regardless of whether ranges are separately disclosed. For example, when a range of "1-5" is disclosed, the described range should be interpreted to include the ranges of "1-4", "1-3", "1-2 and 4-5", "1-3 and 5", and the like. When a numerical range is described herein, unless otherwise indicated, the range is intended to include its endpoints and all integers and fractions within the range.
For the purpose of making the objects, technical solutions and advantages of the present invention more apparent, the technical solutions of the present invention will be clearly and completely described below, and it is apparent that the described embodiments are some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Unless specifically indicated, the technical means used in the embodiments of the present invention are conventional means well known to those skilled in the art. Materials and reagents used in the examples of the present invention are available from regular commercial sources unless otherwise specified.
The bulk density of the 0.2-1mm alumina hollow spheres used in the examples of the present invention was 0.7-0.9g/cm 3 The method comprises the steps of carrying out a first treatment on the surface of the The particle size of the alumina powder is less than 50 mu m.
Example 1
The embodiment provides an alumina refractory material which comprises the following components in percentage by weight: 40% of 0.2-1mm alumina hollow spheres, 50% of micron-sized spherical hollow powder, 5% of alumina powder and 5% of a binding agent (aluminum sulfate).
Wherein, the raw materials of the micron-sized spherical hollow powder are 95 percent of alumina and 5 percent of silica by mass, the particle diameter (D50) is 100 mu m, a plurality of closed small cavities are arranged in the hollow powder, the average diameter of the small cavities is 15 mu m, the average wall thickness of the small cavities is 3 mu m, the whole porosity is 50 percent, the surface pore size is 4 mu m, and the microscopic morphology is shown in figure 1. The stacking density of the micron-sized spherical hollow powder is 0.6g/cm 3 The thermal conductivity was 0.15W/(mK).
The embodiment also provides a preparation method of the alumina refractory material, which comprises the following steps:
step one, preparing a binding agent and water into an aqueous solution with the concentration of 5% for later use;
step two, adding the alumina hollow spheres, the micron-sized spherical hollow powder and the alumina powder into a mixer for uniform stirring;
step three, adding the aqueous solution of the binding agent prepared in the step one into a mixer after stirring for 6 hours, and continuously stirring for 1 hour;
step four, placing the prepared mixture into a die for compression vibration molding, and placing the molded green body into an oven for drying for 24 hours;
and fifthly, placing the dried green body into a muffle furnace for sintering to obtain a product, wherein the sintering temperature is 1600 ℃.
The preparation method of the micron-sized spherical hollow powder comprises the following steps:
s1: preparing powder raw materials and water into slurry, wherein the mass fraction of the powder raw materials in the slurry is 30%, and grinding the slurry in a grinding machine at a rotating speed of 800rpm for 24 hours until the particle size of the powder is 1-10 mu m; preferably 1-5 μm.
S2: dividing the ground slurry in the step S1 into two parts of slurry A and slurry B according to a mass ratio of 1:10, adding PVA with a mass fraction of 2% into the slurry A, adding SAS with a mass fraction of 1%, stirring at a high speed for 20 minutes, wherein the stirring speed is 1000rpm, and forming foam slurry C, wherein the diameter of foam is 0.05-0.3mm; CMC with a mass fraction of 2% and AES with a mass fraction of 1.5% were added to the slurry B, and the mixture was stirred at a high speed of 1500rpm for 60 minutes to form a foam slurry D with an average foam diameter of 15. Mu.m.
S3: and mixing and uniformly stirring the foam slurry C and the foam slurry D for 40min at a stirring speed of 800rpm.
S4: and (3) conveying the foam slurry into a forming tower by using a diaphragm pump, wherein the inlet temperature of the forming tower is 350 ℃, the outlet temperature of the forming tower is 120 ℃, an atomizing disc is arranged in the forming tower, and the rotating speed of the atomizing disc is 9500rpm, so that a spherical hollow powder blank body is obtained.
S5: sintering the green body at 1400 ℃, and cooling to obtain the micron-sized spherical hollow powder.
Example 2
The embodiment provides an alumina refractory material which comprises the following components in percentage by weight: 50% of 0.2-1mm alumina hollow spheres, 40% of micron-sized spherical hollow powder, 8% of alumina powder and 2% of a binding agent (carboxymethyl cellulose).
Wherein the raw materials of the micron-sized spherical hollow powder comprise 95% of alumina and 5% of silicon dioxide by mass, the particle diameter (D50) is 100 μm, and a plurality of closed small parts are arranged insideThe average diameter of the small cavities is 20 mu m, the average wall thickness of the small cavities is 2 mu m, the whole porosity is 60%, and the surface pore size is 2 mu m. The stacking density of the micron-sized spherical hollow powder is 0.5g/cm 3 The thermal conductivity was 0.1W/(mK).
The embodiment also provides a preparation method of the alumina refractory material, which comprises the following steps:
step one, preparing a binding agent and water into an aqueous solution with the concentration of 1.5% for later use;
step two, adding the alumina hollow spheres, the micron-sized spherical hollow powder and the alumina powder into a mixer for uniform stirring;
step three, stirring for 3 hours, and then adding the aqueous solution of the binding agent prepared in the step one into a mixer to continuously stir for 3 hours;
step four, placing the prepared mixture into a die for compression vibration molding, and placing the molded green body into an oven for drying for 36 hours;
and fifthly, placing the dried green body into a muffle furnace for sintering to obtain a product, wherein the sintering temperature is 1600 ℃.
The preparation method of the micron-sized spherical hollow powder comprises the following steps:
s1: preparing a slurry from the powder raw materials and water, wherein the mass fraction of the powder raw materials in the slurry is 30%, and grinding the slurry in a grinder at 800rpm for 24 hours until the particle size of the powder is 1-10 mu m, preferably 1.5-2.5 mu m.
S2: dividing the ground slurry in the step S1 into two parts of slurry A and slurry B according to a mass ratio of 1:10, adding PVA with a mass fraction of 2% into the slurry A, adding SAS with a mass fraction of 1%, stirring at a high speed for 20 minutes, wherein the stirring speed is 1000rpm, and forming foam slurry C, wherein the diameter of foam is 0.05-0.3mm; CMC with the mass fraction of 2% and AES with the mass fraction of 2% are added into the slurry B, and the mixture is stirred at a high speed for 60 minutes, wherein the stirring speed is 1600rpm, so that foam slurry D is formed, and the average diameter of foam is 20 mu m.
S3: and mixing and uniformly stirring the foam slurry C and the foam slurry D for 40min at a stirring speed of 800rpm.
S4: and (3) conveying the foam slurry into a forming tower by using a diaphragm pump, wherein the inlet temperature of the forming tower is 350 ℃, the outlet temperature of the forming tower is 120 ℃, an atomizing disc is arranged in the forming tower, and the rotating speed of the atomizing disc is 9500rpm, so that a spherical hollow powder blank body is obtained.
S5: sintering the green body at 1400 ℃, and cooling to obtain the micron-sized spherical hollow powder.
Example 3
The embodiment provides an alumina refractory material which comprises the following components in percentage by weight: 43% of 0.2-1mm alumina hollow spheres, 44% of micron-sized spherical hollow powder, 5% of alumina powder and 8% of a binding agent (aluminum dihydrogen phosphate).
Wherein, the raw materials of the micron-sized spherical hollow powder are 95 percent of alumina and 5 percent of silica by mass, the particle diameter (D50) is 100 mu m, a plurality of closed small cavities are arranged in the hollow powder, the average diameter of the small cavities is 5 mu m, the average wall thickness of the small cavities is 5 mu m, the whole porosity is 30 percent, and the surface pore size is 3 mu m. The stacking density of the micron-sized spherical hollow powder is 0.8g/cm 3 The thermal conductivity was 0.2W/(mK).
The embodiment also provides a preparation method of the alumina refractory material, which comprises the following steps:
step one, preparing a binding agent and water into an aqueous solution with the concentration of 10% for later use;
step two, adding the alumina hollow spheres, the micron-sized spherical hollow powder and the alumina powder into a mixer for uniform stirring;
step three, adding the aqueous solution of the binding agent prepared in the step one into a mixer after stirring for 6 hours, and continuously stirring for 3 hours;
step four, placing the prepared mixture into a die for compression vibration molding, and placing the molded green body into an oven for drying for 36 hours;
and fifthly, placing the dried green body into a muffle furnace for sintering to obtain a product, wherein the sintering temperature is 1700 ℃.
The preparation method of the micron-sized spherical hollow powder comprises the following steps:
s1: preparing a slurry from the powder raw material and water, wherein the mass fraction of the powder raw material in the slurry is 30%, and grinding the slurry in a grinder at a rotating speed of 800rpm for 24 hours until the particle size of the powder is 1-10 mu m, preferably 3-7 mu m.
S2: dividing the ground slurry in the step S1 into two parts of slurry A and slurry B according to a mass ratio of 1:10, adding PVA with a mass fraction of 2% into the slurry A, adding SAS with a mass fraction of 1%, stirring at a high speed for 20 minutes, wherein the stirring speed is 1000rpm, and forming foam slurry C, wherein the diameter of foam is 0.05-0.3mm; CMC with the mass fraction of 2% and AES with the mass fraction of 0.5% are added to the slurry B, and the mixture is stirred at a high speed for 60 minutes at a stirring speed of 1300rpm to form foam slurry D, wherein the average diameter of foam is 5 mu m.
S3: and mixing and uniformly stirring the foam slurry C and the foam slurry D for 40min at a stirring speed of 800rpm.
S4: and (3) conveying the foam slurry into a forming tower by using a diaphragm pump, wherein the inlet temperature of the forming tower is 350 ℃, the outlet temperature of the forming tower is 120 ℃, an atomizing disc is arranged in the forming tower, and the rotating speed of the atomizing disc is 9500rpm, so that a spherical hollow powder blank body is obtained.
S5: sintering the green body at 1400 ℃, and cooling to obtain the micron-sized spherical hollow powder.
Example 4
The embodiment provides an alumina refractory material which comprises the following components in percentage by weight: 45% of 0.2-1mm alumina hollow spheres, 45% of micron-sized spherical hollow powder, 5% of alumina powder and 5% of a binding agent (aluminum sulfate).
Wherein, the raw materials of the micron-sized spherical hollow powder are 95 percent of alumina and 5 percent of silica by mass, the particle diameter (D50) is 100 mu m, a plurality of closed small cavities are arranged in the hollow powder, the diameter of each small cavity is 12 mu m, the average wall thickness of each small cavity is 3.6 mu m, the whole porosity is 43 percent, and the surface pore size is 5 mu m. The stacking density of the micron-sized spherical hollow powder is 0.68g/cm 3 The thermal conductivity was 0.18W/(mK).
The embodiment also provides a preparation method of the alumina refractory material, which comprises the following steps:
step one, preparing a binding agent and water into an aqueous solution with the concentration of 6% for later use;
step two, adding the alumina hollow spheres, the micron-sized spherical hollow powder and the alumina powder into a mixer for uniform stirring;
step three, adding the aqueous solution of the binding agent prepared in the step one into a mixer after stirring for 6 hours, and continuously stirring for 2 hours;
step four, placing the prepared mixture into a die for compression vibration molding, and placing the molded green body into an oven for drying for 30 hours;
and fifthly, placing the dried green body into a muffle furnace for sintering to obtain a product, wherein the sintering temperature is 1650 ℃.
The preparation method of the micron-sized spherical hollow powder comprises the following steps:
s1: preparing a slurry from the powder raw material and water, wherein the mass fraction of the powder raw material in the slurry is 30%, and grinding the slurry in a grinder at a rotating speed of 800rpm for 24 hours until the particle size of the powder is 1-10 mu m, preferably 2.5-5 mu m.
S2: dividing the ground slurry in the step S1 into two parts of slurry A and slurry B according to a mass ratio of 1:10, adding PVA with a mass fraction of 2% into the slurry A, adding SAS with a mass fraction of 1%, stirring at a high speed for 20 minutes, wherein the stirring speed is 1000rpm, and forming foam slurry C, wherein the diameter of foam is 0.05-0.3mm; CMC in an amount of 2% by mass and AES in an amount of 1.2% by mass were added to the slurry B, and the mixture was stirred at a high speed of 1450rpm for 60 minutes to form a foam slurry D having an average foam diameter of 12. Mu.m.
S3: and mixing and uniformly stirring the foam slurry C and the foam slurry D for 40min at a stirring speed of 800rpm.
S4: and (3) conveying the foam slurry into a forming tower by using a diaphragm pump, wherein the inlet temperature of the forming tower is 350 ℃, the outlet temperature of the forming tower is 120 ℃, an atomizing disc is arranged in the forming tower, and the rotating speed of the atomizing disc is 9500rpm, so that a spherical hollow powder blank body is obtained.
S5: sintering the green body at 1400 ℃, and cooling to obtain the micron-sized spherical hollow powder.
Comparative example 1
The comparative example provides a composition consisting of the following components in weight percent: 40% of 0.2-1mm alumina hollow spheres, 50% of micron-sized spherical hollow powder, 5% of alumina powder and 5% of a binding agent (aluminum sulfate).
Wherein, the raw materials of the micron-sized spherical hollow powder are 95 percent of alumina and 5 percent of silica by mass, the particle diameter (D50) is 100 mu m, a plurality of closed small cavities are arranged in the hollow powder, the average diameter of the small cavities is 25 mu m, the average wall thickness of the small cavities is 1.5 mu m, the whole porosity is 75 percent, and the surface pore size is 4.5 mu m. The stacking density of the micron-sized spherical hollow powder is 0.4g/cm 3 The thermal conductivity was 0.09W/(mK).
Comparative example 2
The comparative example provides an alumina refractory material consisting of the following components in percentage by weight: 20% of 0.2-1mm alumina hollow spheres, 70% of micron-sized spherical hollow powder, 5% of alumina powder and 5% of a binding agent (aluminum sulfate). Wherein the raw materials, the sizes and the preparation methods of the micron-sized spherical hollow powder are the same as in example 1. The alumina refractory was prepared in the same manner as in example 1.
Comparative example 3
The comparative example provides an alumina refractory material consisting of the following components in percentage by weight: 70% of 0.2-1mm alumina hollow spheres, 20% of micron-sized spherical hollow powder, 5% of alumina powder and 5% of a binding agent (aluminum sulfate). Wherein the raw materials, the sizes and the preparation methods of the micron-sized spherical hollow powder are the same as in example 1. The alumina refractory was prepared in the same manner as in example 1.
Comparative example 4
The comparative example provides an alumina refractory material consisting of the following components in percentage by weight: 45% of 0.2-1mm alumina hollow sphere, 50% of alumina powder and 5% of binding agent (aluminum sulfate).
The preparation steps of the alumina refractory material are as follows:
step one, preparing a binding agent and water into an aqueous solution with the concentration of 6% for later use;
step two, adding the alumina hollow spheres and the alumina powder into a mixer for uniform stirring;
step three, adding the aqueous solution of the binding agent prepared in the step one into a mixer after stirring for 6 hours, and continuously stirring for 2 hours;
step four, placing the prepared mixture into a die for compression vibration molding, and placing the molded green body into an oven for drying for 30 hours;
and fifthly, placing the dried green body into a muffle furnace for sintering to obtain a product, wherein the sintering temperature is 1650 ℃.
Comparative example 5
The comparative example provides a composition consisting of the following components in weight percent: 40% of 0.2-1mm alumina hollow spheres, 50% of micron-sized spherical hollow powder, 5% of alumina powder and 5% of a binding agent (aluminum sulfate).
Wherein, the raw materials of the micron-sized spherical hollow powder are 95 percent of alumina and 5 percent of silica by mass, the particle diameter (D50) is 100 mu m, the inside of the powder is provided with a single large cavity, the average shell thickness of the powder is 7 mu m, the whole porosity is 80 percent, and the surface pore size is 8 mu m.
The preparation method of the micron-sized spherical hollow powder comprises the following steps:
s1: taking Al with the mass ratio of 95:5 2 O 3 Powder and SiO 2 Mixing the powder uniformly, and preparing slurry with water; the mass fraction of the powder raw material is about 40%, the mass fraction of the water is about 60%, and the slurry is ground in a grinder at 1500rpm for 48 hours until the particle size of the powder is 3-10 mu m.
S2: to the ground slurry, 2% PVA by mass and 1% AES by mass were added, and the mixture was stirred at a high speed of 1500rpm for 60 minutes to form a foam slurry, wherein the average diameter of the foam was 0.09mm.
S3: and conveying the foam slurry into a closed reaction kettle, carrying out aging reaction for 8 hours at 40 ℃, and stirring at a stirring speed of 150rpm.
S4: and (3) conveying the foam slurry into a forming tower by using a diaphragm pump, wherein the inlet temperature of the forming tower is 300 ℃, the outlet temperature of the forming tower is 150 ℃, an atomizing disk is arranged in the forming tower, the rotating speed of the atomizing disk is 10000rpm, and a spherical hollow powder blank body with the diameter (D50) of 100 mu m and the water content of 0.5% is obtained.
S5: and (3) loading the spherical hollow powder blank obtained in the step (S4) into a sagger, placing the sagger into a muffle furnace for sintering, wherein the sintering temperature is 1400 ℃, the heat preservation time is 2h, and cooling the sagger to room temperature along with the furnace to obtain the spherical hollow powder.
Performance testing
The alumina refractories obtained in the above examples and comparative examples were subjected to performance tests. The test items comprise density, strength and heat conductivity, wherein the strength detection method refers to GB/T5072-2008 refractory material normal temperature compressive strength test method, the heat conductivity detection method refers to international standard ISO22007-2, and the results are shown in the following table.
TABLE 1
Project | Density g/cm 3 | Strength MPa | Thermal conductivity W/(m.K) |
Example 1 | 1.09 | 11.2 | 0.254 |
Example 2 | 1.13 | 12.5 | 0.279 |
Example 3 | 1.26 | 15.6 | 0.297 |
Example 4 | 1.19 | 13.1 | 0.282 |
Comparative example 1 | 0.98 | 4.5 | 0.153 |
Comparative example 2 | 1.01 | 5.8 | 0.174 |
Comparative example 3 | 1.35 | 22.4 | 0.495 |
Comparative example 4 | 1.55 | 37.5 | 1.455 |
Comparative example 5 | 0.95 | 4.4 | 0.142 |
From the results, the alumina refractory material prepared by the invention has the advantages of low density, light weight and low heat conductivity coefficient on the premise of meeting the strength use requirement, thereby having better heat preservation effect and saving energy.
Finally, it should be noted that: the above embodiments are only for illustrating the technical solution of the present invention, and are not limiting; although the invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical scheme described in the foregoing embodiments can be modified or some technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit and scope of the technical solutions of the embodiments of the present invention.
Claims (8)
1. An alumina refractory material is characterized by comprising the following components in percentage by weight: 40-50% of 0.2-1mm alumina hollow spheres, 40-50% of micron-sized spherical hollow powder, 5-15% of alumina powder and 1.5-10% of binding agent;
wherein, the micron-sized spherical hollow powder is internally provided with a plurality of closed small cavities, and the overall porosity is 30-60%;
the particle size of the micron-sized spherical hollow powder is 50-150 mu m, the surface pore size is 2-5 mu m, and the average diameter of the small cavity is 5-20 mu m; the average wall thickness of the small cavity is 2-5 mu m;
the preparation method of the micron-sized spherical hollow powder comprises the following steps:
s1: preparing slurry from the powder raw materials and water, and grinding to obtain powder with a granularity of 1-10 μm;
s2: dividing the ground slurry in the step S1 into two parts of slurry A and slurry B, adding a first binder and a first surfactant into the slurry A, and uniformly stirring to obtain foam slurry C with the diameter of 0.05-0.3mm; adding a second binder and a second surfactant into the slurry B, and uniformly stirring to obtain foam slurry D with the diameter of 5-50 mu m;
s3: mixing and uniformly stirring the foam slurry C and the foam slurry D obtained in the step S2;
s4: carrying out atomization molding on the product obtained in the step S3 in a molding tower to obtain a spherical hollow powder blank;
and S5, sintering the spherical hollow powder blank obtained in the step S4, and cooling to obtain the spherical hollow powder.
2. The alumina refractory according to claim 1, wherein the raw material of the micron-sized spherical hollow powder comprises 80% or more of alumina by mass.
3. The alumina refractory according to claim 2, wherein the raw material of the micron-sized spherical hollow powder is composed of 90-95% by mass of alumina and 5-10% by mass of silica.
4. The alumina refractory according to claim 2, wherein the micron-sized spherical hollow powder has a bulk density of 0.5 to 0.8g/cm 3 The heat conductivity coefficient is 0.1-0.2W/(mK).
5. The alumina refractory of any one of claims 1-4, wherein the alumina refractory meets one or more of the following conditions:
a. the bulk density of the alumina hollow sphere with 0.2-1mm is 0.7-0.9g/cm 3 ;
b. The granularity of the alumina powder is less than 50 mu m;
c. the binding agent is one or more of aluminum sulfate, aluminum dihydrogen phosphate, epoxy resin and carboxymethyl cellulose.
6. A method for producing an alumina refractory according to any one of claims 1 to 5, comprising: the components are mixed, formed, dried and sintered, wherein the sintering temperature is 1600-1700 ℃.
7. The method of producing an alumina refractory according to claim 6, wherein the binder is mixed with water to prepare an aqueous solution having a concentration of 1.5 to 10% and then with the remaining components.
8. A refractory article comprising the alumina refractory material of any one of claims 1-5.
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