CN115304386A - Mullite composite refractory brick and processing technology thereof - Google Patents
Mullite composite refractory brick and processing technology thereof Download PDFInfo
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- CN115304386A CN115304386A CN202211068679.9A CN202211068679A CN115304386A CN 115304386 A CN115304386 A CN 115304386A CN 202211068679 A CN202211068679 A CN 202211068679A CN 115304386 A CN115304386 A CN 115304386A
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- 239000011449 brick Substances 0.000 title claims abstract description 89
- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 title claims abstract description 81
- 229910052863 mullite Inorganic materials 0.000 title claims abstract description 81
- 239000002131 composite material Substances 0.000 title claims abstract description 46
- 238000005516 engineering process Methods 0.000 title claims abstract description 10
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims abstract description 90
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims abstract description 84
- 239000006087 Silane Coupling Agent Substances 0.000 claims abstract description 49
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims abstract description 47
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 43
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims abstract description 37
- 239000004606 Fillers/Extenders Substances 0.000 claims abstract description 33
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims abstract description 33
- 239000004927 clay Substances 0.000 claims abstract description 31
- 239000007864 aqueous solution Substances 0.000 claims abstract description 30
- INAHAJYZKVIDIZ-UHFFFAOYSA-N boron carbide Chemical compound B12B3B4C32B41 INAHAJYZKVIDIZ-UHFFFAOYSA-N 0.000 claims abstract description 30
- 229910052580 B4C Inorganic materials 0.000 claims abstract description 29
- 239000004793 Polystyrene Substances 0.000 claims abstract description 29
- 229920002223 polystyrene Polymers 0.000 claims abstract description 29
- 235000006408 oxalic acid Nutrition 0.000 claims abstract description 28
- 239000006004 Quartz sand Substances 0.000 claims abstract description 27
- 239000002070 nanowire Substances 0.000 claims abstract description 16
- 229910010271 silicon carbide Inorganic materials 0.000 claims abstract description 16
- 238000003763 carbonization Methods 0.000 claims abstract description 9
- 238000013329 compounding Methods 0.000 claims abstract description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 81
- 239000000203 mixture Substances 0.000 claims description 47
- 239000008367 deionised water Substances 0.000 claims description 45
- 229910021641 deionized water Inorganic materials 0.000 claims description 45
- 238000009210 therapy by ultrasound Methods 0.000 claims description 33
- 238000003756 stirring Methods 0.000 claims description 30
- 238000010304 firing Methods 0.000 claims description 20
- 238000002156 mixing Methods 0.000 claims description 17
- 239000013589 supplement Substances 0.000 claims description 16
- 238000004321 preservation Methods 0.000 claims description 15
- 239000011265 semifinished product Substances 0.000 claims description 12
- 238000001035 drying Methods 0.000 claims description 11
- 238000000034 method Methods 0.000 claims description 9
- 238000000748 compression moulding Methods 0.000 claims description 8
- 239000000377 silicon dioxide Substances 0.000 claims description 7
- 239000002994 raw material Substances 0.000 claims description 6
- 239000000919 ceramic Substances 0.000 claims description 5
- 230000008569 process Effects 0.000 claims description 5
- 150000001875 compounds Chemical class 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 4
- 238000001914 filtration Methods 0.000 claims description 4
- 238000003825 pressing Methods 0.000 claims description 4
- 235000012239 silicon dioxide Nutrition 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 4
- 238000005303 weighing Methods 0.000 claims description 4
- 229910010293 ceramic material Inorganic materials 0.000 claims description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 8
- 229910052799 carbon Inorganic materials 0.000 abstract description 8
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 abstract description 7
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 abstract description 7
- 239000005011 phenolic resin Substances 0.000 abstract description 7
- 229920001568 phenolic resin Polymers 0.000 abstract description 7
- 238000005452 bending Methods 0.000 abstract description 6
- 230000004048 modification Effects 0.000 abstract description 6
- 238000012986 modification Methods 0.000 abstract description 6
- 230000035939 shock Effects 0.000 abstract description 4
- 230000009471 action Effects 0.000 abstract description 3
- 238000011065 in-situ storage Methods 0.000 abstract description 3
- 238000006116 polymerization reaction Methods 0.000 abstract description 3
- 230000002035 prolonged effect Effects 0.000 abstract description 3
- 230000000052 comparative effect Effects 0.000 description 12
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 4
- 229910052796 boron Inorganic materials 0.000 description 4
- 239000007791 liquid phase Substances 0.000 description 4
- 238000000465 moulding Methods 0.000 description 4
- 239000012071 phase Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 230000004888 barrier function Effects 0.000 description 2
- 239000007767 bonding agent Substances 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 229910052593 corundum Inorganic materials 0.000 description 2
- 239000010431 corundum Substances 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 229910052500 inorganic mineral Inorganic materials 0.000 description 2
- 239000004973 liquid crystal related substance Substances 0.000 description 2
- 239000011707 mineral Substances 0.000 description 2
- 230000006911 nucleation Effects 0.000 description 2
- 238000010899 nucleation Methods 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 1
- KMWBBMXGHHLDKL-UHFFFAOYSA-N [AlH3].[Si] Chemical class [AlH3].[Si] KMWBBMXGHHLDKL-UHFFFAOYSA-N 0.000 description 1
- CSDREXVUYHZDNP-UHFFFAOYSA-N alumanylidynesilicon Chemical compound [Al].[Si] CSDREXVUYHZDNP-UHFFFAOYSA-N 0.000 description 1
- 239000002199 base oil Substances 0.000 description 1
- JJWKPURADFRFRB-UHFFFAOYSA-N carbonyl sulfide Chemical compound O=C=S JJWKPURADFRFRB-UHFFFAOYSA-N 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000011451 fired brick Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 239000011819 refractory material Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000011452 unfired brick Substances 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
Classifications
-
- 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
- C04B35/66—Monolithic refractories or refractory mortars, including those whether or not containing clay
-
- 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
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/34—Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3418—Silicon oxide, silicic acids or oxide forming salts thereof, e.g. silica sol, fused silica, silica fume, cristobalite, quartz or flint
-
- 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
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/34—Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3427—Silicates other than clay, e.g. water glass
- C04B2235/3463—Alumino-silicates other than clay, e.g. mullite
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- 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
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/34—Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/349—Clays, e.g. bentonites, smectites such as montmorillonite, vermiculites or kaolines, e.g. illite, talc or sepiolite
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/38—Non-oxide ceramic constituents or additives
- C04B2235/3817—Carbides
- C04B2235/3821—Boron carbides
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/38—Non-oxide ceramic constituents or additives
- C04B2235/3817—Carbides
- C04B2235/3826—Silicon carbides
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
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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
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- C04B2235/9607—Thermal properties, e.g. thermal expansion coefficient
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- Compositions Of Oxide Ceramics (AREA)
- Ceramic Products (AREA)
Abstract
The invention discloses a mullite composite refractory brick and a processing technology thereof, wherein the mullite composite refractory brick comprises quartz sand, clay, polystyrene, mullite and an extender. The invention can effectively enhance the bending strength and the fracture toughness, and can effectively enhance the anti-seismic performance of the mullite composite refractory brick, so that the mullite refractory brick is not easy to damage in use, and the service life is prolonged; carrying out surface modification treatment on the silicon carbide nanowires under the action of a silane coupling agent; phenol, formaldehyde aqueous solution and oxalic acid react to generate a layer of smooth phenolic resin through in-situ polymerization on the surface of the silicon carbide nanowire, the silicon carbide nanowire coated with the carbon layer is formed after carbonization treatment, and the silicon carbide nanowire is added into the refractory brick to be compounded with alumina, so that the bending strength and the fracture toughness of the refractory brick can be effectively improved, and the anti-seismic performance of the refractory brick is further enhanced; the boron carbide and the silica sol are added into the refractory brick in a compounding way, so that the growth of a mullite phase is facilitated, the volume expansion is generated, and the thermal shock resistance of the refractory brick can be effectively improved.
Description
Technical Field
The invention relates to the technical field of refractory bricks, in particular to a mullite composite refractory brick and a processing technology thereof.
Background
The refractory bricks are called fire bricks for short; mainly made of refractory clay or other refractory materials. The refractory bricks can be divided into fired bricks, unfired bricks, fused cast bricks and refractory heat-insulating bricks according to the preparation process; depending on the composition of the refractory brick, it can be divided into five main categories, namely: silicon-aluminum series refractory bricks, alkaline series refractory bricks, carbon-containing refractory bricks, zirconium-containing refractory bricks and heat-insulating refractory bricks. The silicon-aluminum refractory brick mainly comprises: silica brick, clay brick, high-alumina refractory brick and corundum refractory brick; the clay brick mainly comprises mullite (25-50%), a glass phase (25-60%), cristobalite and quartz (30% at most); the mineral composition of the high-alumina refractory brick comprises corundum, mullite and a glass phase.
But the existing mullite refractory brick has poor anti-seismic performance, so that the mullite refractory brick is easy to damage in use, and the service life is shortened.
Disclosure of Invention
In order to overcome the defects in the prior art, the embodiment of the invention provides a mullite composite refractory brick and a processing technology thereof.
A mullite composite refractory brick comprises the following components in percentage by weight: 13.6 to 14.6 percent of quartz sand, 17.6 to 18.6 percent of clay, 17.4 to 18.4 percent of polystyrene, 16.5 to 16.9 percent of extender and the balance of mullite.
Further, the supplement comprises the following components in percentage by weight: 6.6 to 7.6 percent of silicon carbide nanowire, 23.6 to 24.6 percent of boron carbide, 0.4 to 0.6 percent of silane coupling agent, 8.2 to 8.8 percent of phenol, 13.6 to 14.6 percent of formaldehyde aqueous solution, 0.7 to 1.1 percent of oxalic acid and the balance of silica sol.
Further, the mullite composite refractory brick comprises the following components in percentage by weight: 13.6% of quartz sand, 17.6% of clay, 17.4% of polystyrene, 16.5% of extender and the balance of mullite; the supplement comprises the following components in percentage by weight: 6.6 percent of silicon carbide nano wire, 23.6 percent of boron carbide, 0.4 percent of silane coupling agent, 8.2 percent of phenol, 13.6 percent of formaldehyde aqueous solution, 0.7 percent of oxalic acid and the balance of silica sol.
Further, the mullite composite refractory brick comprises the following components in percentage by weight: 14.6% of quartz sand, 18.6% of clay, 18.4% of polystyrene, 16.9% of extender and the balance of mullite; the supplement comprises the following components in percentage by weight: 7.6 percent of silicon carbide nano wire, 24.6 percent of boron carbide, 0.6 percent of silane coupling agent, 8.8 percent of phenol, 14.6 percent of formaldehyde aqueous solution, 1.1 percent of oxalic acid and the balance of silica sol.
Further, the mullite composite refractory brick comprises the following components in percentage by weight: 14.1% of quartz sand, 18.1% of clay, 17.9% of polystyrene, 16.7% of extender and the balance of mullite; the supplement comprises the following components in percentage by weight: 7.1 percent of silicon carbide nano wire, 24.1 percent of boron carbide, 0.5 percent of silane coupling agent, 8.5 percent of phenol, 14.1 percent of formaldehyde aqueous solution, 0.9 percent of oxalic acid and the balance of silica sol.
Further, the silane coupling agent is prepared by compounding one or more of a silane coupling agent KH-550, a silane coupling agent KH-560 and a silane coupling agent KH-570; the purity of the formaldehyde aqueous solution is 37-38%; the content of silicon dioxide in the silica sol is 30-40%.
A processing technology of mullite composite refractory brick comprises the following specific processing steps:
the method comprises the following steps: weighing quartz sand, clay, polystyrene, mullite in the raw materials of the impregnating compound and silicon carbide nanowires, boron carbide, a silane coupling agent, phenol, a formaldehyde aqueous solution, oxalic acid and silica sol in the extender;
step two: adding the silane coupling agent in the step one into deionized water, carrying out ultrasonic treatment for 20-30 minutes, adding the silicon carbide nanowire in the step one, continuing the ultrasonic treatment for 40-60 minutes, and carrying out centrifugal filtration treatment to obtain a mixture A;
step three: adding the phenol and formaldehyde aqueous solution in the step one into deionized water, carrying out water bath ultrasonic treatment for 20-30 minutes, adding the mixture A in the step two and the oxalic acid in the step one, continuing the water bath ultrasonic treatment for 110-130 minutes, carrying out water bath heat preservation and stirring treatment for 3-5 hours, cooling, washing and drying, and carrying out carbonization treatment at the temperature of 260-280 ℃ to obtain a mixture B;
step four: blending the mixture B in the third step with the boron carbide and the silica sol in the first step to obtain the extender;
step five: adding the polystyrene in the step one and the extender in the step four into deionized water, and performing blending ultrasonic treatment for 20-30 minutes to obtain a mixture C;
step six: adding the quartz sand, the clay and the mullite in the step one into the mixture C in the step five, blending and stirring for 40-60 minutes, and performing ultrasonic treatment for 20-30 minutes to obtain a mixture D;
step seven: pressing and forming the mixture D in the sixth step to obtain a semi-finished product;
step eight: and drying the semi-finished product in the sixth step, and then firing and molding to obtain the mullite composite refractory brick.
Further, in the second step, the weight ratio of the silane coupling agent to the deionized water is 1: 80-100, the ultrasonic frequency is 60-80 KHz, and the ultrasonic power is 800-900W; in the third step, the weight ratio of the phenol to the deionized water is 1: 10-20, the water bath temperature is 55-65 ℃, the ultrasonic frequency is 60-80 KHz, the ultrasonic power is 800-900W, the water bath heat preservation temperature is 80-90 ℃, and the stirring speed is 500-700 r/min; in the fifth step, the weight ratio of the replenisher to the deionized water is 1: 10-20, the ultrasonic frequency is 1.4-1.6 MHz, and the ultrasonic power is 300-400W; in the sixth step, the stirring speed is 300-500 r/min, the ultrasonic frequency is 1.4-1.6 MHz, and the ultrasonic power is 300-400W; in the seventh step, the pressure of the compression molding is 80-90 MPa; in the step eight, the drying treatment is carried out for 21 to 27 hours at the temperature of between 55 and 65 ℃, and the firing forming is carried out for 11 to 13 hours at the temperature of between 1400 and 1500 ℃.
Further, in the second step, the weight ratio of the silane coupling agent to the deionized water is 1: 80, the ultrasonic frequency is 60KHz, and the ultrasonic power is 800W; in the third step, the weight ratio of the phenol to the deionized water is 1: 10, the water bath temperature is 55 ℃, the ultrasonic frequency is 60KHz, the ultrasonic power is 800W, the water bath heat preservation temperature is 80 ℃, and the stirring speed is 500r/min; in the fifth step, the weight ratio of the replenisher to the deionized water is 1: 10, the ultrasonic frequency is 1.4MHz, and the ultrasonic power is 300W; in the sixth step, the stirring speed is 300r/min, the ultrasonic frequency is 1.4MHz, and the ultrasonic power is 300W; in the seventh step, the pressure of the compression molding is 80MPa; in step eight, the ceramic is dried at 55 ℃ for 21 hours, and the firing forming is specifically firing at 1400 ℃ for 11 hours.
Further, in the second step, the weight ratio of the silane coupling agent to the deionized water is 1: 90, the ultrasonic frequency is 70KHz, and the ultrasonic power is 850W; in the third step, the weight ratio of the phenol to the deionized water is 1: 15, the water bath temperature is 60 ℃, the ultrasonic frequency is 70KHz, the ultrasonic power is 850W, the water bath heat preservation temperature is 85 ℃, and the stirring speed is 600r/min; in the fifth step, the weight ratio of the replenisher to the deionized water is 1: 15, the ultrasonic frequency is 1.5MHz, and the ultrasonic power is 350W; in the sixth step, the stirring speed is 400r/min, the ultrasonic frequency is 1.5MHz, and the ultrasonic power is 350W; in the seventh step, the pressure of the compression molding is 85MPa; in step eight, the ceramic is dried for 24 hours at 60 ℃, and the firing forming is specifically firing for 12 hours at 1450 ℃.
The invention has the technical effects and advantages that:
1. the mullite composite refractory brick processed by the raw material formula can effectively enhance the bending strength and the fracture toughness, and effectively enhance the shock resistance of the mullite composite refractory brick, so that the mullite refractory brick is not easy to damage in use, and the service life is prolonged; polystyrene is added into the refractory brick, a large amount of nano-scale closed pores can be generated in the sintering process, the thermal conductivity is low, and the refractory performance of the refractory brick is ensured; the silicon carbide nanowires in the replenisher are subjected to surface modification treatment under the action of a silane coupling agent, and hydrophilic groups are grafted on the surfaces of the silicon carbide nanowires, so that the follow-up surface coating modification treatment of phenolic resin is facilitated; phenol, formaldehyde aqueous solution and oxalic acid in the replenisher react to generate a layer of smooth phenolic resin through in-situ polymerization on the surface of the silicon carbide nanowire, the silicon carbide nanowire coated with the carbon layer is formed after carbonization treatment, the silicon carbide nanowire coated with the carbon layer is added into the refractory brick to be compounded with alumina, the bending strength and the fracture toughness of the refractory brick can be effectively improved, and the anti-seismic performance of the refractory brick is further enhanced; boron carbide and silica sol in the extender are compounded, the silica sol is used as a bonding agent and added into the refractory brick, the boron carbide is added into the refractory brick to promote the generation of a boron-rich liquid phase, and crystal grains of alumina and silica are wetted by the boron-rich liquid phase, so that a crystal grain interface has a small nucleation barrier, the growth of a mullite phase is facilitated, the volume expansion is generated, and the thermal shock resistance of the refractory brick can be effectively improved;
2. in the second step, the silane coupling agent is added into deionized water for ultrasonic treatment, and then the silicon carbide nanowires are added, so that the silane coupling agent and the silicon carbide nanowires can be effectively subjected to rapid reaction composite treatment, and the surface grafting treatment effect of the silicon carbide nanowires is ensured; in the third step, phenol and formaldehyde aqueous solution are added into deionized water, water bath ultrasonic treatment is carried out, then the mixture A and oxalic acid are added, the water bath ultrasonic treatment and the water bath heat preservation treatment are continued, phenolic resin can be effectively coated on the surface of the silicon carbide nano wire, and the subsequent carbonization treatment is carried out, so that the silicon carbide nano wire coated with the carbon layer can be effectively prepared; in the fourth step, the mixture B is blended with boron carbide and silica sol to form the extender; in the fifth step, adding the polystyrene and the extender into deionized water, and performing blending ultrasonic treatment to obtain a mixture C; in the sixth step, quartz sand, clay and mullite are added into the mixture C, and the mixture D is obtained through blending, stirring and ultrasonic treatment; in the seventh step, the mixture D is pressed and formed to obtain a semi-finished product; and step eight, drying the semi-finished product, and then firing and molding to obtain the mullite composite refractory brick.
Detailed Description
The following will clearly and completely describe the technical solutions in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1:
the invention provides a mullite composite refractory brick, which comprises the following components in percentage by weight: 13.6% of quartz sand, 17.6% of clay, 17.4% of polystyrene, 16.5% of extender and the balance of mullite; the supplement comprises the following components in percentage by weight: 6.6 percent of silicon carbide nanowire, 23.6 percent of boron carbide, 0.4 percent of silane coupling agent, 8.2 percent of phenol, 13.6 percent of formaldehyde aqueous solution, 0.7 percent of oxalic acid and the balance of silica sol;
the silane coupling agent is a silane coupling agent KH-560; the purity of the formaldehyde aqueous solution is 37-38%; the content of silicon dioxide in the silica sol is 30-40%;
quartz sand was purchased from America Source cosmic renewable resources, inc., grade: the first grade, the model is 20-40 meshes; the clay is purchased from 325 mesh clay of Xucheng mineral product processing factory in Lingshu county; polystyrene was purchased from the commercial company, ltd, and no: GPPS-251; mullite was purchased from zheng next sail refractory limited, specifications: 200 meshes; the silicon carbide nanowires are purchased from Guangzhou Hongwu materials science and technology Co., ltd, CAS number 409-21-2; boron carbide was purchased from Shandong jin Shengtai chemical Co., ltd., CAS number: 12069-32-8, model: industrial grade; the silane coupling agent KH-560 was purchased from Wuhan Poov Biotech, inc., cat #: 0002 of a base oil; phenol was purchased from shin-jin-shun chemical limited, CAS:108-95-2, grade: a superior product; the formaldehyde aqueous solution is purchased from Didization engineering Co., ltd, huainan city, and has a purity of 37.4%; oxalic acid was purchased from the chemical technology ltd of shiteng, hubei, cat #: 032563; the silica sol was purchased from Jinxin resources and chemical Co., ltd, and had a silica content of 35%, a pH of 8.5 and a viscosity (25 ℃ C.): 5.0;
the invention also provides a processing technology of the mullite composite refractory brick, which comprises the following specific processing steps:
the method comprises the following steps: weighing quartz sand, clay, polystyrene, mullite in the raw materials of the impregnating compound and silicon carbide nanowires, boron carbide, a silane coupling agent, phenol, a formaldehyde aqueous solution, oxalic acid and silica sol in the extender;
step two: adding the silane coupling agent in the step one into deionized water, carrying out ultrasonic treatment for 20 minutes, adding the silicon carbide nanowire in the step one, continuing the ultrasonic treatment for 40 minutes, and carrying out centrifugal filtration treatment to obtain a mixture A;
step three: adding the phenol and formaldehyde aqueous solution in the step one into deionized water, carrying out water bath ultrasonic treatment for 20 minutes, adding the mixture A in the step two and the oxalic acid in the step one, continuing the water bath ultrasonic treatment for 110 minutes, carrying out water bath heat preservation stirring treatment for 3 hours, cooling, washing, drying, and then carrying out carbonization treatment at the temperature of 260 ℃ to obtain a mixture B;
step four: blending the mixture B in the third step with the boron carbide and the silica sol in the first step to obtain the extender;
step five: adding the polystyrene in the step one and the extender in the step four into deionized water, and blending and ultrasonically treating for 20 minutes to obtain a mixture C;
step six: adding the quartz sand, the clay and the mullite in the step one into the mixture C in the step five, blending and stirring for 40 minutes, and performing ultrasonic treatment for 20 minutes to obtain a mixture D;
step seven: pressing and forming the mixture D in the sixth step to obtain a semi-finished product;
step eight: and drying the semi-finished product in the sixth step, and then firing and molding to obtain the mullite composite refractory brick.
In the second step, the weight ratio of the silane coupling agent to the deionized water is 1: 80, the ultrasonic frequency is 60KHz, and the ultrasonic power is 800W; in the third step, the weight ratio of the phenol to the deionized water is 1: 10, the water bath temperature is 55 ℃, the ultrasonic frequency is 60KHz, the ultrasonic power is 800W, the water bath heat preservation temperature is 80 ℃, and the stirring speed is 500r/min; in the fifth step, the weight ratio of the replenisher to the deionized water is 1: 10, the ultrasonic frequency is 1.4MHz, and the ultrasonic power is 300W; in the sixth step, the stirring speed is 300r/min, the ultrasonic frequency is 1.4MHz, and the ultrasonic power is 300W; in the seventh step, the pressure of the press forming is 80MPa; in step eight, the ceramic is dried at 55 ℃ for 21 hours, and the firing forming is specifically firing at 1400 ℃ for 11 hours.
Example 2:
different from the embodiment 1, the mullite composite refractory brick comprises the following components in percentage by weight: 14.6% of quartz sand, 18.6% of clay, 18.4% of polystyrene, 16.9% of extender and the balance of mullite; the supplement comprises the following components in percentage by weight: 7.6 percent of silicon carbide nano wire, 24.6 percent of boron carbide, 0.6 percent of silane coupling agent, 8.8 percent of phenol, 14.6 percent of formaldehyde aqueous solution, 1.1 percent of oxalic acid and the balance of silica sol.
Example 3:
different from the examples 1-2, the mullite composite refractory brick comprises the following components in percentage by weight: 14.1% of quartz sand, 18.1% of clay, 17.9% of polystyrene, 16.7% of extender and the balance of mullite; the supplement comprises the following components in percentage by weight: 7.1 percent of silicon carbide nano wire, 24.1 percent of boron carbide, 0.5 percent of silane coupling agent, 8.5 percent of phenol, 14.1 percent of formaldehyde aqueous solution, 0.9 percent of oxalic acid and the balance of silica sol.
Example 4:
different from the embodiment 3, in the second step, the weight ratio of the silane coupling agent to the deionized water is 1: 100, the ultrasonic frequency is 80KHz, and the ultrasonic power is 900W; in the third step, the weight ratio of the phenol to the deionized water is 1: 20, the water bath temperature is 65 ℃, the ultrasonic frequency is 80KHz, the ultrasonic power is 900W, the water bath heat preservation temperature is 90 ℃, and the stirring speed is 700r/min; in the fifth step, the weight ratio of the replenisher to the deionized water is 1: 20, the ultrasonic frequency is 1.6MHz, and the ultrasonic power is 400W; in the sixth step, the stirring speed is 500r/min, the ultrasonic frequency is 1.6MHz, and the ultrasonic power is 400W; in the seventh step, the pressure of the compression molding is 90MPa; in step eight, the ceramic is dried at 65 ℃ for 27 hours, and the firing forming is specifically firing at 1500 ℃ for 13 hours.
Example 5:
different from the embodiment 3, in the second step, the weight ratio of the silane coupling agent to the deionized water is 1: 90, the ultrasonic frequency is 70KHz, and the ultrasonic power is 850W; in the third step, the weight ratio of the phenol to the deionized water is 1: 15, the water bath temperature is 60 ℃, the ultrasonic frequency is 70KHz, the ultrasonic power is 850W, the water bath heat preservation temperature is 85 ℃, and the stirring speed is 600r/min; in the fifth step, the weight ratio of the replenisher to the deionized water is 1: 15, the ultrasonic frequency is 1.5MHz, and the ultrasonic power is 350W; in the sixth step, the stirring speed is 400r/min, the ultrasonic frequency is 1.5MHz, and the ultrasonic power is 350W; in the seventh step, the pressure of the compression molding is 85MPa; in the step eight, the ceramic material is dried at 60 ℃ for 24 hours, and the firing forming is carried out at 1450 ℃ for 12 hours.
Example 6:
different from the embodiment 5, the processing technology of the mullite composite refractory brick comprises the following specific processing steps:
the method comprises the following steps: weighing quartz sand, clay, polystyrene, mullite in the raw materials of the impregnating compound and silicon carbide nanowires, boron carbide, a silane coupling agent, phenol, a formaldehyde aqueous solution, oxalic acid and silica sol in the extender;
step two: adding the silane coupling agent in the step one into deionized water, carrying out ultrasonic treatment for 25 minutes, adding the silicon carbide nanowire in the step one, continuing ultrasonic treatment for 50 minutes, and carrying out centrifugal filtration treatment to obtain a mixture A;
step three: adding the phenol and formaldehyde aqueous solution in the step one into deionized water, carrying out water bath ultrasonic treatment for 25 minutes, adding the mixture A in the step two and the oxalic acid in the step one, continuing the water bath ultrasonic treatment for 120 minutes, carrying out water bath heat preservation stirring treatment for 4 hours, cooling, washing, drying, and carrying out carbonization treatment at the temperature of 270 ℃ to obtain a mixture B;
step four: blending the mixture B in the third step with the boron carbide and the silica sol in the first step to obtain the extender;
step five: adding the polystyrene in the step one and the extender in the step four into deionized water, and carrying out blending ultrasonic treatment for 25 minutes to obtain a mixture C;
step six: adding the quartz sand, the clay and the mullite in the step one into the mixture C in the step five, blending and stirring for 50 minutes, and performing ultrasonic treatment for 25 minutes to obtain a mixture D;
step seven: pressing and forming the mixture D in the sixth step to obtain a semi-finished product;
step eight: and sixthly, drying the semi-finished product in the step six, and then firing and forming to obtain the mullite composite refractory brick.
Comparative example 1:
the difference from example 3 is: the mullite composite refractory brick comprises the following components in percentage by weight: 14.1 percent of quartz sand, 18.1 percent of clay, 17.9 percent of polystyrene and the balance of mullite.
Comparative example 2:
the difference from example 3 is: the mullite composite refractory brick comprises the following components in percentage by weight: 14.1% of quartz sand, 18.1% of clay, 17.9% of polystyrene, 16.7% of extender and the balance of mullite; the supplement comprises the following components in percentage by weight: 24.1 percent of boron carbide, 0.5 percent of silane coupling agent, 8.5 percent of phenol, 14.1 percent of formaldehyde aqueous solution, 0.9 percent of oxalic acid and the balance of silica sol.
Comparative example 3:
the difference from example 3 is: the mullite composite refractory brick comprises the following components in percentage by weight: 14.1% of quartz sand, 18.1% of clay, 17.9% of polystyrene, 16.7% of extender and the balance of mullite; the supplement comprises the following components in percentage by weight: 7.1 percent of silicon carbide nano wire, 0.5 percent of silane coupling agent, 8.5 percent of phenol, 14.1 percent of formaldehyde aqueous solution, 0.9 percent of oxalic acid and the balance of silica sol.
Comparative example 4:
the difference from example 5 is: the mullite composite refractory brick comprises the following components in percentage by weight: 14.1% of quartz sand, 18.1% of clay, 17.9% of polystyrene, 16.7% of extender and the balance of mullite; the supplement comprises the following components in percentage by weight: 7.1 percent of silicon carbide nano wire, 24.1 percent of boron carbide, 0.5 percent of silane coupling agent, 0.9 percent of oxalic acid and the balance of silica sol.
Comparative example 5:
the difference from example 5 is: blending and stirring all the raw materials of the supplement for 3 hours to obtain the supplement; the stirring speed is 400r/min.
The mullite composite refractory brick in the comparative example and the embodiment of the invention is detected; the mullite composite refractory bricks in the examples and the comparative examples are tested for fracture toughness according to the GB9341-1988 standard; the results are shown in table one:
table one:
| fracture toughness value (MPa. M) 1/2 ) | |
| Comparative example 1 | 4.84 |
| Comparative example 2 | 5.21 |
| Comparative example 3 | 5.32 |
| Comparative example 4 | 5.22 |
| Comparative example 5 | 5.36 |
| Example 1 | 5.68 |
| Example 2 | 5.64 |
| Example 3 | 5.77 |
| Example 4 | 5.73 |
| Example 5 | 5.85 |
| Example 6 | 5.87 |
From the above table, it can be seen that: the mullite composite refractory brick can effectively enhance the bending strength and the fracture toughness, and effectively enhance the anti-seismic performance of the mullite composite refractory brick, so that the mullite refractory brick is not easy to damage in use, and the service life of the mullite composite refractory brick is prolonged.
The polystyrene is added into the refractory brick, so that a large amount of nano-scale closed pores can be generated in the sintering process, the thermal conductivity is low, and the refractory performance of the refractory brick is ensured; the silicon carbide nanowires in the replenisher are subjected to surface modification treatment under the action of a silane coupling agent, and hydrophilic groups are grafted on the surfaces of the silicon carbide nanowires, so that the follow-up surface coating modification treatment of phenolic resin is facilitated; phenol, formaldehyde aqueous solution and oxalic acid in the replenisher react to generate a layer of smooth phenolic resin through in-situ polymerization on the surface of the silicon carbide nanowire, the silicon carbide nanowire coated with the carbon layer is formed after carbonization treatment, the silicon carbide nanowire coated with the carbon layer is added into the refractory brick to be compounded with alumina, the bending strength and the fracture toughness of the refractory brick can be effectively improved, and the anti-seismic performance of the refractory brick is further enhanced; boron carbide and silica sol in the extender are compounded, the silica sol is used as a bonding agent and added into the refractory brick, the boron carbide is added into the refractory brick to promote the generation of a boron-rich liquid phase, and crystal grains of alumina and silica are wetted by the boron-rich liquid phase, so that a crystal grain interface has a small nucleation barrier, the growth of a mullite phase is facilitated, the volume expansion is generated, and the thermal shock resistance of the refractory brick can be effectively improved; in the second step, the silane coupling agent is added into deionized water for ultrasonic treatment, and then the silicon carbide nanowires are added, so that the silane coupling agent and the silicon carbide nanowires can be effectively subjected to rapid reaction composite treatment, and the surface grafting treatment effect of the silicon carbide nanowires is ensured; in the third step, phenol and formaldehyde aqueous solution are added into deionized water, water bath ultrasonic treatment is carried out, then the mixture A and oxalic acid are added, the water bath ultrasonic treatment and the water bath heat preservation treatment are continued, phenolic resin can be effectively coated on the surface of the silicon carbide nanowire, and the subsequent carbonization treatment is carried out, so that the silicon carbide nanowire coated with the carbon layer can be effectively prepared; in the fourth step, the mixture B is blended with boron carbide and silica sol to form the extender; in the fifth step, adding the polystyrene and the extender into deionized water, and performing blending ultrasonic treatment to obtain a mixture C; in the sixth step, quartz sand, clay and mullite are added into the mixture C, and the mixture D is obtained through blending, stirring and ultrasonic treatment; in the seventh step, the mixture D is pressed and formed to obtain a semi-finished product; and step eight, drying the semi-finished product, and then firing and molding to obtain the mullite composite refractory brick.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that changes may be made in the embodiments and/or equivalents thereof without departing from the spirit and scope of the invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A mullite composite refractory brick is characterized in that: comprises the following components in percentage by weight: 13.6 to 14.6 percent of quartz sand, 17.6 to 18.6 percent of clay, 17.4 to 18.4 percent of polystyrene, 16.5 to 16.9 percent of extender and the balance of mullite.
2. The mullite composite refractory brick as set forth in claim 1, wherein: the supplement comprises the following components in percentage by weight: 6.6 to 7.6 percent of silicon carbide nanowire, 23.6 to 24.6 percent of boron carbide, 0.4 to 0.6 percent of silane coupling agent, 8.2 to 8.8 percent of phenol, 13.6 to 14.6 percent of formaldehyde aqueous solution, 0.7 to 1.1 percent of oxalic acid and the balance of silica sol.
3. The mullite composite refractory brick as set forth in claim 2, wherein: the weight percentage of the components is as follows: 13.6% of quartz sand, 17.6% of clay, 17.4% of polystyrene, 16.5% of extender and the balance of mullite; the supplement comprises the following components in percentage by weight: 6.6 percent of silicon carbide nano wire, 23.6 percent of boron carbide, 0.4 percent of silane coupling agent, 8.2 percent of phenol, 13.6 percent of formaldehyde aqueous solution, 0.7 percent of oxalic acid and the balance of silica sol.
4. The mullite composite refractory brick as set forth in claim 2, wherein: comprises the following components in percentage by weight: 14.6% of quartz sand, 18.6% of clay, 18.4% of polystyrene, 16.9% of extender and the balance of mullite; the supplement comprises the following components in percentage by weight: 7.6 percent of silicon carbide nano wire, 24.6 percent of boron carbide, 0.6 percent of silane coupling agent, 8.8 percent of phenol, 14.6 percent of formaldehyde aqueous solution, 1.1 percent of oxalic acid and the balance of silica sol.
5. The mullite composite refractory brick as claimed in claim 2, wherein: the weight percentage of the components is as follows: 14.1% of quartz sand, 18.1% of clay, 17.9% of polystyrene, 16.7% of extender and the balance of mullite; the supplement comprises the following components in percentage by weight: 7.1 percent of silicon carbide nano wire, 24.1 percent of boron carbide, 0.5 percent of silane coupling agent, 8.5 percent of phenol, 14.1 percent of formaldehyde aqueous solution, 0.9 percent of oxalic acid and the balance of silica sol.
6. The mullite composite refractory brick as claimed in claim 1, wherein: the silane coupling agent is prepared by compounding one or more of a silane coupling agent KH-550, a silane coupling agent KH-560 and a silane coupling agent KH-570; the purity of the formaldehyde aqueous solution is 37-38%; the content of silicon dioxide in the silica sol is 30-40%.
7. A processing technology of mullite composite refractory brick is characterized in that: the specific processing steps are as follows:
the method comprises the following steps: weighing quartz sand, clay, polystyrene, mullite in the raw materials of the impregnating compound and silicon carbide nanowires, boron carbide, a silane coupling agent, phenol, a formaldehyde aqueous solution, oxalic acid and silica sol in the extender;
step two: adding the silane coupling agent in the step one into deionized water, carrying out ultrasonic treatment for 20-30 minutes, adding the silicon carbide nanowire in the step one, continuing the ultrasonic treatment for 40-60 minutes, and carrying out centrifugal filtration treatment to obtain a mixture A;
step three: adding the phenol and formaldehyde aqueous solution in the step one into deionized water, carrying out water bath ultrasonic treatment for 20-30 minutes, adding the mixture A in the step two and the oxalic acid in the step one, continuing the water bath ultrasonic treatment for 110-130 minutes, carrying out water bath heat preservation and stirring treatment for 3-5 hours, cooling, washing and drying, and carrying out carbonization treatment at the temperature of 260-280 ℃ to obtain a mixture B;
step four: blending the mixture B in the third step with the boron carbide and the silica sol in the first step to obtain the extender;
step five: adding the polystyrene in the step one and the extender in the step four into deionized water, and performing blending ultrasonic treatment for 20-30 minutes to obtain a mixture C;
step six: adding the quartz sand, the clay and the mullite in the step one into the mixture C in the step five, blending and stirring for 40-60 minutes, and performing ultrasonic treatment for 20-30 minutes to obtain a mixture D;
step seven: pressing and forming the mixture D in the sixth step to obtain a semi-finished product;
step eight: and sixthly, drying the semi-finished product in the step six, and then firing and forming to obtain the mullite composite refractory brick.
8. The process of claim 7, wherein the mullite composite refractory brick comprises the following steps: in the second step, the weight ratio of the silane coupling agent to the deionized water is 1: 80-100, the ultrasonic frequency is 60-80 KHz, and the ultrasonic power is 800-900W; in the third step, the weight ratio of the phenol to the deionized water is 1: 10-20, the water bath temperature is 55-65 ℃, the ultrasonic frequency is 60-80 KHz, the ultrasonic power is 800-900W, the water bath heat preservation temperature is 80-90 ℃, and the stirring speed is 500-700 r/min; in the fifth step, the weight ratio of the replenisher to the deionized water is 1: 10-20, the ultrasonic frequency is 1.4-1.6 MHz, and the ultrasonic power is 300-400W; in the sixth step, the stirring speed is 300-500 r/min, the ultrasonic frequency is 1.4-1.6 MHz, and the ultrasonic power is 300-400W; in the seventh step, the pressure of the compression molding is 80-90 MPa; in the step eight, the mixture is dried for 21 to 27 hours at the temperature of between 55 and 65 ℃, and the firing forming is specifically fired for 11 to 13 hours at the temperature of between 1400 and 1500 ℃.
9. The process of claim 8, wherein the mullite composite refractory brick comprises: in the second step, the weight ratio of the silane coupling agent to the deionized water is 1: 80, the ultrasonic frequency is 60KHz, and the ultrasonic power is 800W; in the third step, the weight ratio of the phenol to the deionized water is 1: 10, the water bath temperature is 55 ℃, the ultrasonic frequency is 60KHz, the ultrasonic power is 800W, the water bath heat preservation temperature is 80 ℃, and the stirring speed is 500r/min; in the fifth step, the weight ratio of the replenisher to the deionized water is 1: 10, the ultrasonic frequency is 1.4MHz, and the ultrasonic power is 300W; in the sixth step, the stirring speed is 300r/min, the ultrasonic frequency is 1.4MHz, and the ultrasonic power is 300W; in the seventh step, the pressure of the compression molding is 80MPa; in step eight, the ceramic is dried at 55 ℃ for 21 hours, and the firing forming is specifically firing at 1400 ℃ for 11 hours.
10. The process of claim 8, wherein the mullite composite refractory brick comprises: in the second step, the weight ratio of the silane coupling agent to the deionized water is 1: 90, the ultrasonic frequency is 70KHz, and the ultrasonic power is 850W; in the third step, the weight ratio of the phenol to the deionized water is 1: 15, the water bath temperature is 60 ℃, the ultrasonic frequency is 70KHz, the ultrasonic power is 850W, the water bath heat preservation temperature is 85 ℃, and the stirring speed is 600r/min; in the fifth step, the weight ratio of the replenisher to the deionized water is 1: 15, the ultrasonic frequency is 1.5MHz, and the ultrasonic power is 350W; in the sixth step, the stirring speed is 400r/min, the ultrasonic frequency is 1.5MHz, and the ultrasonic power is 350W; in the seventh step, the pressure of the compression molding is 85MPa; in the step eight, the ceramic material is dried at 60 ℃ for 24 hours, and the firing forming is carried out at 1450 ℃ for 12 hours.
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