CN114671692A - Double-layer high-strength heat-preservation refractory castable and preparation method thereof - Google Patents
Double-layer high-strength heat-preservation refractory castable and preparation method thereof Download PDFInfo
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- CN114671692A CN114671692A CN202210450294.2A CN202210450294A CN114671692A CN 114671692 A CN114671692 A CN 114671692A CN 202210450294 A CN202210450294 A CN 202210450294A CN 114671692 A CN114671692 A CN 114671692A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 59
- 238000004321 preservation Methods 0.000 title claims abstract description 24
- 239000002245 particle Substances 0.000 claims abstract description 111
- 239000000843 powder Substances 0.000 claims abstract description 91
- 239000002131 composite material Substances 0.000 claims abstract description 55
- 239000003094 microcapsule Substances 0.000 claims abstract description 55
- 238000002156 mixing Methods 0.000 claims abstract description 48
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 40
- 239000000919 ceramic Substances 0.000 claims abstract description 40
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 39
- CSDREXVUYHZDNP-UHFFFAOYSA-N alumanylidynesilicon Chemical compound [Al].[Si] CSDREXVUYHZDNP-UHFFFAOYSA-N 0.000 claims abstract description 38
- 239000000463 material Substances 0.000 claims abstract description 32
- 229910010271 silicon carbide Inorganic materials 0.000 claims abstract description 31
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims abstract description 30
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 29
- 230000003014 reinforcing effect Effects 0.000 claims abstract description 28
- 239000010703 silicon Substances 0.000 claims abstract description 25
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 25
- 239000002994 raw material Substances 0.000 claims abstract description 19
- 229910052751 metal Inorganic materials 0.000 claims abstract description 18
- 239000002184 metal Substances 0.000 claims abstract description 18
- 239000004568 cement Substances 0.000 claims abstract description 17
- 229910052593 corundum Inorganic materials 0.000 claims abstract description 17
- 239000010431 corundum Substances 0.000 claims abstract description 16
- 239000010426 asphalt Substances 0.000 claims abstract description 14
- 239000002270 dispersing agent Substances 0.000 claims abstract description 14
- 239000011863 silicon-based powder Substances 0.000 claims abstract description 14
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 11
- 239000010410 layer Substances 0.000 claims description 125
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 26
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 claims description 25
- 239000000920 calcium hydroxide Substances 0.000 claims description 25
- 229910001861 calcium hydroxide Inorganic materials 0.000 claims description 25
- 239000011268 mixed slurry Substances 0.000 claims description 23
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 22
- 238000001035 drying Methods 0.000 claims description 21
- 239000011248 coating agent Substances 0.000 claims description 18
- 238000000576 coating method Methods 0.000 claims description 18
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims description 16
- 239000005011 phenolic resin Substances 0.000 claims description 16
- 229920001568 phenolic resin Polymers 0.000 claims description 16
- 239000000945 filler Substances 0.000 claims description 14
- 239000012044 organic layer Substances 0.000 claims description 14
- 238000009210 therapy by ultrasound Methods 0.000 claims description 14
- JPUHCPXFQIXLMW-UHFFFAOYSA-N aluminium triethoxide Chemical compound CCO[Al](OCC)OCC JPUHCPXFQIXLMW-UHFFFAOYSA-N 0.000 claims description 13
- 239000004927 clay Substances 0.000 claims description 13
- 239000007788 liquid Substances 0.000 claims description 13
- 210000001161 mammalian embryo Anatomy 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 10
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 10
- 238000001914 filtration Methods 0.000 claims description 10
- 238000000034 method Methods 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 5
- VGGLHLAESQEWCR-UHFFFAOYSA-N N-(hydroxymethyl)urea Chemical compound NC(=O)NCO VGGLHLAESQEWCR-UHFFFAOYSA-N 0.000 claims description 5
- 229910052799 carbon Inorganic materials 0.000 claims description 5
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 5
- 239000000377 silicon dioxide Substances 0.000 claims description 5
- 235000012239 silicon dioxide Nutrition 0.000 claims description 5
- 238000002791 soaking Methods 0.000 claims description 5
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 5
- WXZMFSXDPGVJKK-UHFFFAOYSA-N pentaerythritol Chemical group OCC(CO)(CO)CO WXZMFSXDPGVJKK-UHFFFAOYSA-N 0.000 claims description 4
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 26
- 229910052742 iron Inorganic materials 0.000 description 13
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 10
- 230000000052 comparative effect Effects 0.000 description 8
- 238000005266 casting Methods 0.000 description 6
- 239000002355 dual-layer Substances 0.000 description 6
- 239000001569 carbon dioxide Substances 0.000 description 5
- 229910002092 carbon dioxide Inorganic materials 0.000 description 5
- 230000007797 corrosion Effects 0.000 description 5
- 238000005260 corrosion Methods 0.000 description 5
- 239000011148 porous material Substances 0.000 description 5
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 4
- 239000004743 Polypropylene Substances 0.000 description 4
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 description 4
- 239000000292 calcium oxide Substances 0.000 description 4
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 4
- 239000000835 fiber Substances 0.000 description 4
- -1 polypropylene Polymers 0.000 description 4
- 229920001155 polypropylene Polymers 0.000 description 4
- 239000002689 soil Substances 0.000 description 4
- 239000006185 dispersion Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 238000010079 rubber tapping Methods 0.000 description 3
- 229910000019 calcium carbonate Inorganic materials 0.000 description 2
- 238000003763 carbonization Methods 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 238000009413 insulation Methods 0.000 description 2
- GCLGEJMYGQKIIW-UHFFFAOYSA-H sodium hexametaphosphate Chemical compound [Na]OP1(=O)OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])O1 GCLGEJMYGQKIIW-UHFFFAOYSA-H 0.000 description 2
- 235000019982 sodium hexametaphosphate Nutrition 0.000 description 2
- 235000019832 sodium triphosphate Nutrition 0.000 description 2
- 239000001577 tetrasodium phosphonato phosphate Substances 0.000 description 2
- 229910000805 Pig iron Inorganic materials 0.000 description 1
- 229910018540 Si C Inorganic materials 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 239000011241 protective layer Substances 0.000 description 1
- 238000009991 scouring Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 229910001845 yogo sapphire Inorganic materials 0.000 description 1
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- 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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/02—Making microcapsules or microballoons
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- C04B33/00—Clay-wares
- C04B33/02—Preparing or treating the raw materials individually or as batches
- C04B33/04—Clay; Kaolin
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- 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
- C04B35/16—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 silicates other than clay
- C04B35/18—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 silicates other than clay rich in aluminium oxide
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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
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
- C04B2235/3208—Calcium oxide or oxide-forming salts thereof, e.g. lime
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- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3217—Aluminum oxide or oxide forming salts thereof, e.g. bauxite, alpha-alumina
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- 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
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- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
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- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/42—Non metallic elements added as constituents or additives, e.g. sulfur, phosphor, selenium or tellurium
- C04B2235/428—Silicon
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- C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
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- C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
- C04B2235/54—Particle size related information
- C04B2235/5418—Particle size related information expressed by the size of the particles or aggregates thereof
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Abstract
The invention relates to a double-layer high-strength heat-preservation refractory castable and a preparation method thereof, wherein the refractory castable comprises an inner-layer castable and an outer-layer castable, the preparation raw materials of the inner-layer castable comprise a first aggregate and a blending material, and the first aggregate comprises a silicon-aluminum aggregate and ceramic reinforcing particles; the preparation raw materials of the outer-layer castable comprise a second aggregate and a blending material, wherein the second aggregate comprises a silicon-aluminum aggregate and composite microcapsule particles; the silicon-aluminum aggregate comprises high-aluminum aggregate, silicon carbide, fine alumina powder, silicon micro powder and white corundum powder; the admixture comprises metal silicon powder, spherical asphalt, cement, an explosion-proof agent and a dispersing agent.
Description
Technical Field
The invention belongs to the technical field of refractory furnace materials, and particularly relates to a double-layer high-strength heat-preservation refractory castable and a preparation method thereof.
Background
The blast furnace is the main equipment for smelting pig iron, the tapping runner is the necessary way for molten iron to flow from the furnace to the molten iron tank, and the quality and performance of the tapping runner are related to the quality of the molten iron and the normal production of the blast furnace. The working environment of the iron runner is severe, the iron runner can be repeatedly washed by high-temperature molten iron, the temperature change is severe, the material requirement of the iron runner is very stable, and the corrosion can be slowed down in the long-term use process.
At present, most of the workers in the field study the iron runner, and study the stability, the scouring resistance and the corrosion resistance of the material of the iron runner, however, the requirement of the iron runner on the strength of the iron runner is higher in the working environment, and the inventor finds that the damage of the iron runner caused by severe temperature change can be effectively relieved by improving the heat insulation performance of the iron runner.
Disclosure of Invention
Aiming at the problems, the invention provides a double-layer high-strength heat-preservation refractory castable and a preparation method thereof, wherein the refractory castable comprises an inner-layer castable and an outer-layer castable, the preparation raw materials of the inner-layer castable comprise a first aggregate and a blending material, and the first aggregate comprises a silicon-aluminum aggregate and ceramic reinforcing particles;
the preparation raw materials of the outer-layer castable comprise a second aggregate and a blending material, wherein the second aggregate comprises a silicon-aluminum aggregate and composite microcapsule particles;
the silicon-aluminum aggregate comprises high-aluminum aggregate, silicon carbide, fine alumina powder, silicon micro powder and white corundum powder; the admixture comprises metal silicon powder, spherical asphalt, cement, an explosion-proof agent and a dispersing agent.
Aiming at the defects of the existing light heat-insulating castable, the invention designs the double-layer refractory castable, the inner-layer castable is directly contacted with furnace burden in an industrial kiln, and the castable has higher strength and better corrosion resistance under the holding of ceramic reinforcing particles; the outer layer casting material is porous light casting material, and has good heat preservation performance. And the silicon-aluminum aggregate and the admixture of the inner-layer castable and the outer-layer castable are the same, namely most components are the same, so that the two layers are ensured to have better binding property and are firmly combined with each other to form a pouring protective layer of the industrial kiln together.
Optionally, the preparation raw materials of the ceramic reinforcing particles comprise silicon-aluminum sol and clay, and the particle size of the ceramic reinforcing particles is 1-3 mm; the mass ratio of the silicon-aluminum sol to the clay is (0.05-0.2): 1.
According to the invention, the ceramic reinforcing particles are added into the first aggregate of the inner-layer castable, the ceramic reinforcing particles can be uniformly dispersed in the first aggregate, and the particles have high strength and good high-temperature and corrosion resistance, so that the strength, the high-temperature and the corrosion resistance of the inner-layer castable are improved. The inventor also unexpectedly finds that the surface substance of the ceramic reinforcing particles in the high-temperature environment can act or react with certain components of the inner-layer castable to strengthen the connection of the ceramic reinforcing particles and other components, and although the inventor has not explored a specific reaction principle, the inventor speculates that Al-Si-C and oxide thereof in the silicon-aluminum aggregate and cement react with the components of the ceramic reinforcing particles at high temperature to generate crystals or whiskers with higher strength, so that the strength and stability of the inner-layer castable are improved.
Optionally, the composite microcapsule particles are spherical, and sequentially include an organic layer, an inorganic layer and an internal filler from outside to inside, the organic layer includes phenolic resin, a carbon forming agent and aluminum ethoxide, the inorganic layer includes silica-alumina sol, and the internal filler includes aluminum powder and/or calcium hydroxide. The particle size of the composite microcapsule particles is 1-5 mm.
Optionally, the carbon forming agent is pentaerythritol, and the mass ratio of the phenolic resin to the carbon forming agent to the aluminum ethoxide is 1 (1.1-1.5) to 0.02-0.12. Preferably, the molecular weight of the phenolic resin is 100-200.
Optionally, the outer layer casting material further comprises a curing agent, the curing agent comprises hydroxymethyl urea and sodium carbonate and is used for curing phenolic resin, and the mass ratio of the phenolic resin to the hydroxymethyl urea to the sodium carbonate is 1 (0.9-2) to 0.6-1.
According to the invention, the composite microcapsule particles are added into the outer-layer castable, and the organic layer of the composite microcapsule particles can play a role of an adhesive during mixing and pouring of the second aggregate and the admixture, so that the composite microcapsule particles, the second aggregate and the admixture are combined more firmly, and when the composite microcapsule particles are used, the organic layer is carbonized to form holes under the high-temperature action of an industrial kiln, and a uniform pore structure is formed inside the outer-layer castable and on the outer layer of the composite microcapsule particles, so that the heat insulation performance is improved. In addition, the aluminum ethoxide added into the organic layer plays a role of a surfactant, so that the uniform dispersion of the composite microcapsule particles in the second aggregate is promoted when the outer-layer castable is prepared, and meanwhile, the aluminum ethoxide is beneficial to uniformly mixing all components of the organic layer per se and promoting the combination of the organic layer and the inorganic layer.
Calcium hydroxide in the internal filler can absorb part of carbon dioxide released during carbonization of the organic layer through pores of the inorganic layer, so that cracking caused by excessive release of carbon dioxide in a short time in the use process of the outer-layer castable is prevented; when the temperature is higher, the inorganic layer is broken, the internal filler is released, namely the aluminum powder, the calcium carbonate and part of unreacted calcium hydroxide are released, wherein the calcium carbonate is decomposed into calcium oxide and carbon dioxide by high heat, which is equivalent to secondary release of the carbon dioxide, the calcium hydroxide is decomposed into calcium oxide and water by high heat, the calcium oxide is matched with the components of the outer-layer castable, the strength of the outer-layer castable is improved, the aluminum powder is oxidized to generate aluminum oxide, and the strength of the outer-layer castable can be further improved.
Optionally, the grain size of the high-alumina aggregate of the inner-layer castable is 5-8mm, the grain size of the silicon carbide is 0.5-1mm, the SiC content in the silicon carbide is not less than 98%, the grain size of the fine alumina powder is 5-8 μm, and Al in the fine alumina powder2O3The content of the silicon dioxide is not less than 87 percent, the grain diameter of the silicon micro powder is 0.1-0.5 mu m, and SiO in the silicon micro powder2The content is not less than 95 percent, and the grain diameter of the white corundum powder is 5-10 mm.
Optionally, the grain size of the high-alumina aggregate of the outer-layer castable is 8-10mm, the grain size of the silicon carbide is 1-2mm, the SiC content in the silicon carbide is not less than 98%, the grain size of the fine alumina powder is 8-15 μm, and Al in the fine alumina powder is Al2O3The content of the silicon micro powder is not less than 87 percent, and the particle size of the silicon micro powder0.5-1.5 μm, SiO in the silicon micropowder2The content is not less than 95 percent, and the grain diameter of the white corundum powder is 5-15 mm.
Optionally, the grain size of the metal silicon powder of the inner-layer castable and the outer-layer castable is 0.1-0.3 μm, the grain size of the spherical asphalt is 0.5-0.9mm, and the cement is high-alumina 80 cement.
Optionally, the explosion-proof agent is metal aluminum powder and polypropylene fiber, the particle size of the metal aluminum powder is 45-55 μm, and the length of the polypropylene fiber is 5-10 mm.
Optionally, the dispersing agent is selected from one or two of sodium hexametaphosphate and sodium tripolyphosphate.
Optionally, the inner layer castable comprises the following raw materials in parts by weight: 50-60 parts of high-aluminum aggregate, 15-25 parts of silicon carbide, 5-7 parts of fine aluminum oxide powder, 3-5 parts of silicon micropowder, 3-5 parts of white corundum powder, 10-18 parts of ceramic reinforced particles, 2-3 parts of metal silicon powder, 2-3 parts of spherical asphalt, 2-3 parts of cement, 0.1-0.2 part of explosion-proof agent and 0.1-0.2 part of dispersing agent.
Optionally, the outer-layer castable comprises the following raw materials in parts by weight: 55-66 parts of high-aluminum aggregate, 10-20 parts of silicon carbide, 5-7 parts of fine aluminum oxide powder, 3-5 parts of silicon micropowder, 3-5 parts of white corundum powder, 10-15 parts of composite microcapsule particles, 2-3 parts of metal silicon powder, 2-3 parts of spherical asphalt, 2-3 parts of cement, 0.1-0.2 part of explosion-proof agent and 0.1-0.2 part of dispersing agent.
The preparation method of the refractory castable material comprises a preparation method of the ceramic reinforcing particles, a preparation method of the composite microcapsule particles, a preparation method of an inner-layer castable material and a preparation method of an outer-layer castable material.
Optionally, the preparation method of the ceramic reinforced particle comprises the following steps:
(1) mixing the silicon-aluminum sol and the clay according to the mass ratio (0.05-0.2) to 1 to obtain first mixed slurry;
(2) filtering the first mixed slurry, and drying at the temperature of 100-120 ℃ to obtain first powder;
(3) and roasting the first powder at the temperature of 900-1200 ℃ for 6-8h to obtain the ceramic reinforced particles.
Optionally, the preparation method of the inner layer castable comprises the following steps:
(4) uniformly mixing the silicon-aluminum aggregate of the inner-layer castable and the ceramic reinforcing particles according to the mass parts to obtain inner-layer premix;
(5) and mixing the inner-layer premix and the blended material according to the mass parts, and uniformly stirring to obtain the inner-layer castable.
Optionally, the preparation method of the composite microcapsule particle includes the following steps:
(6) mixing aluminum powder and calcium hydroxide powder with equal mass with the silicon-aluminum sol, and performing ultrasonic treatment to uniformly disperse the mixture to obtain second mixed slurry;
(7) filtering the second mixed slurry and drying at the temperature of 100-120 ℃ to obtain second powder;
(8) roasting the second powder at the temperature of 500-700 ℃ for 5-6h to obtain a prefabricated blank, soaking the prefabricated blank in water for 0.5-1h, and then drying at the temperature of 30-50 ℃ to obtain a blank;
(9) dissolving phenolic resin and aluminum ethoxide in the mass ratio of 1 (0.02-0.12) in ethanol, and uniformly mixing to obtain a coating solution;
(10) and (4) immersing the embryo body obtained in the step (8) into the coating liquid, carrying out ultrasonic treatment for 10-20min, taking out the embryo body with the coating liquid on the surface, and drying at room temperature to remove ethanol to obtain the composite microcapsule particles with wet surfaces.
Optionally, the preparation method of the outer castable comprises the following steps:
(11) uniformly mixing silicon-aluminum aggregate of the outer-layer castable, adding the composite microcapsule particles, uniformly mixing, and uniformly mixing a curing agent to obtain an outer-layer premix;
(12) and mixing the outer-layer premix and the blended material according to the mass parts, and uniformly stirring to obtain the outer-layer castable.
In the step (8), calcium hydroxide inside the second powder after being roasted is decomposed, so that the prefabricated blank is immersed in water, water enters the prefabricated blank through the pores of the inorganic layer and reacts with calcium oxide to generate calcium hydroxide, and carbon dioxide can be absorbed conveniently in the subsequent use process.
Preferably, in the step (6), aluminum powder and the silicon-aluminum sol are mixed, and are subjected to ultrasonic treatment and uniform dispersion to obtain a third mixed slurry, and calcium hydroxide powder and the silicon-aluminum sol are mixed, and are subjected to ultrasonic treatment and uniform dispersion to obtain a fourth mixed slurry; wherein the aluminum powder and the calcium hydroxide powder have the same mass;
in the step (7), the third mixed slurry is filtered and dried at the temperature of 100-;
in the step (8), the third powder and the fourth powder are respectively roasted at 500 ℃ for 6 hours to respectively obtain a first blank and a second prefabricated blank, then the second prefabricated blank is soaked in water for 0.5 hour, and then dried at 30 ℃ to obtain a second blank;
and (10) immersing the first embryo body and the second embryo body with equal mass into the coating liquid, performing ultrasonic treatment for 20min, taking out the embryo body with the coating liquid on the surface, and drying at room temperature to remove ethanol to obtain the composite microcapsule particles with wet surfaces.
Because the aluminum powder is hydrated in water, the aluminum powder and the calcium hydroxide powder can be respectively filled in the inorganic layer, and only the composite microcapsule particles filled with the calcium hydroxide powder are soaked in water, so that the composite microcapsule particles filled with the aluminum powder are protected.
Detailed Description
Example 1
The double-layer high-strength heat-preservation refractory castable disclosed by the embodiment comprises an inner-layer castable and an outer-layer castable, wherein the inner-layer castable comprises a first aggregate and a blending material, and the first aggregate comprises a silicon-aluminum aggregate and ceramic reinforcing particles;
the preparation raw materials of the outer-layer castable comprise a second aggregate and a blending material, wherein the second aggregate comprises a silicon-aluminum aggregate and composite microcapsule particles;
the silicon-aluminum aggregate comprises high-aluminum aggregate, silicon carbide, fine alumina powder, silicon micropowder and white corundum powder; the admixture comprises metal silicon powder, spherical asphalt, cement, an explosion-proof agent and a dispersing agent.
The preparation raw materials of the ceramic reinforced particles comprise silicon-aluminum sol and clay, and the particle size of the ceramic reinforced particles is 1-3 mm; the mass ratio of the silica-alumina sol to the clay is 0.05: 1.
The composite microcapsule particles are spherical and sequentially comprise an organic layer, an inorganic layer and an internal filler from outside to inside, the components of the organic layer comprise phenolic resin (CAS number is 9003-35-4), pentaerythritol and aluminum ethoxide, the components of the inorganic layer comprise silica-alumina sol, and the internal filler comprises aluminum powder and/or calcium hydroxide. The particle size of the composite microcapsule particles is 1 mm.
The outer-layer castable also comprises a curing agent, wherein the curing agent comprises hydroxymethyl urea and sodium carbonate, and the mass ratio of the phenolic resin to the hydroxymethyl urea to the sodium carbonate is 1:0.9: 0.6.
The grain size of the high-alumina aggregate of the inner-layer castable is 5-8mm, the grain size of the silicon carbide is 0.5-1mm, the SiC content in the silicon carbide is not lower than 98%, the grain size of the alumina fine powder is 5-8 mu m, and Al in the alumina fine powder2O3The content of the silicon dioxide is not less than 87 percent, the grain diameter of the silicon micro powder is 0.1-0.5 mu m, and SiO in the silicon micro powder2The content is not less than 95 percent, and the grain diameter of the white corundum powder is 5-10 mm.
The grain size of the high-alumina aggregate of the outer-layer castable is 8-10mm, the grain size of the silicon carbide is 1-2mm, the SiC content in the silicon carbide is not lower than 98%, the grain size of the alumina fine powder is 8-15 mu m, and the Al content in the alumina fine powder is2O3The content of the silicon dioxide is not less than 87 percent, the grain diameter of the silicon micro powder is 0.5 to 1.5 mu m, and SiO in the silicon micro powder2The content is not less than 95 percent, and the grain diameter of the white corundum powder is 5-15 mm.
The grain diameter of the metal silicon powder of the inner layer casting material and the outer layer casting material is 0.1-0.3 mu m, the grain diameter of the spherical asphalt is 0.5-0.9mm, and the cement is high-alumina 80 cement.
The explosion-proof agent is metal aluminum powder and polypropylene fiber with the same mass, the particle size of the metal aluminum powder is 45-55 mu m, and the length of the polypropylene fiber is 5-10 mm.
The dispersing agent is sodium hexametaphosphate and sodium tripolyphosphate which have the same mass.
The inner layer castable comprises the following raw materials in parts by weight: 50 parts of high-alumina aggregate, 15 parts of silicon carbide, 5 parts of alumina fine powder, 3 parts of silicon micropowder, 3 parts of white corundum powder, 10 parts of ceramic reinforcing particles, 2 parts of metal silicon powder, 2 parts of spherical asphalt, 2 parts of cement, 0.1 part of explosion-proof agent and 0.1 part of dispersing agent.
The outer-layer castable comprises the following raw materials in parts by weight: 55 parts of high-aluminum aggregate, 10 parts of silicon carbide, 5 parts of fine alumina powder, 3 parts of silicon micropowder, 3 parts of white corundum powder, 10 parts of composite microcapsule particles, 2 parts of metal silicon powder, 2 parts of spherical asphalt, 2 parts of cement, 0.1 part of explosion-proof agent and 0.1 part of dispersing agent.
The preparation method of the refractory castable material in this embodiment includes a preparation method of the ceramic reinforcing particles, a preparation method of the composite microcapsule particles, a preparation method of the inner castable material, and a preparation method of the outer castable material.
The preparation method of the ceramic reinforced particle comprises the following steps:
(1) mixing silicon-aluminum sol and clay according to the mass ratio of 0.05:1 to obtain first mixed slurry;
(2) filtering the first mixed slurry, and drying at 100 ℃ to obtain first powder;
(3) and roasting the first powder at 900 ℃ for 8 hours to obtain the ceramic reinforced particles.
The preparation method of the inner layer castable comprises the following steps:
(4) uniformly mixing the silicon-aluminum aggregate of the inner-layer castable and the ceramic reinforcing particles according to the mass parts to obtain an inner-layer premix;
(5) and mixing the inner-layer premix and the blended material according to the mass parts, and uniformly stirring to obtain the inner-layer castable.
The preparation method of the composite microcapsule particles comprises the following steps:
(6) mixing aluminum powder and calcium hydroxide powder with equal mass with the silicon-aluminum sol, and performing ultrasonic treatment to uniformly disperse the mixture to obtain second mixed slurry;
(7) filtering the second mixed slurry and drying at 100 ℃ to obtain second powder;
(8) roasting the second powder at 500 ℃ for 6h to obtain a prefabricated blank, soaking the prefabricated blank in water for 0.5h, and then drying at 30 ℃ to obtain a blank;
(9) dissolving phenolic resin, pentaerythritol and aluminum ethoxide in ethanol according to the mass ratio of 1:1:0.02, and uniformly mixing to obtain a coating solution;
(10) and (4) immersing the embryo body obtained in the step (8) into the coating liquid, carrying out ultrasonic treatment for 20min, taking out the embryo body with the coating liquid on the surface, and drying at room temperature to remove ethanol to obtain the composite microcapsule particles with wet surfaces.
The preparation method of the outer-layer castable comprises the following steps:
(11) uniformly mixing the silicon-aluminum aggregate of the outer-layer castable, adding the composite microcapsule particles, uniformly mixing, adding the curing agent, and uniformly mixing to obtain an outer-layer premix;
(12) and mixing the outer-layer premix and the blended material according to the mass parts, and uniformly stirring to obtain the outer-layer castable.
Comparative example 1
The double-layer high-strength heat-preservation refractory castable in the comparative example is the same as that in example 1, except that the inner-layer castable does not contain ceramic reinforcing particles, and the outer-layer castable does not contain composite microcapsule particles and a curing agent.
The preparation method of the inner layer castable comprises the following steps: (1) uniformly mixing the silicon-aluminum aggregate of the inner-layer castable according to the mass part of the embodiment 1 to obtain inner-layer premix; (2) and (2) mixing the inner-layer premix and the blended material according to the mass part of the embodiment 1, and uniformly stirring to obtain an inner-layer castable.
The preparation method of the outer-layer castable comprises the following steps: (1) uniformly mixing the silicon-aluminum aggregate of the outer-layer castable according to the mass part of the embodiment 1 to obtain an outer-layer premix; (2) and (3) mixing the outer-layer premix and the blended material according to the mass parts in the embodiment 1, and uniformly stirring to obtain an outer-layer castable.
Example 2
The double-layer high-strength heat-preservation refractory castable and the preparation method thereof in the embodiment are the same as those in the embodiment 1, and the difference is that the ceramic reinforcing particles are prepared from silicon-aluminum sol and common sandy soil.
The preparation method of the ceramic reinforced particle of the embodiment comprises the following steps:
(1) mixing the silicon-aluminum sol and common sandy soil according to the mass ratio of 0.05:1 to obtain first mixed slurry;
(2) filtering the first mixed slurry, and drying at 100 ℃ to obtain first powder;
(3) the first powder was calcined at 900 ℃ for 8 hours to obtain ceramic reinforcing particles of the present example.
Example 3
The double-layer high-strength heat-preservation refractory castable and the preparation method thereof in this embodiment are the same as those in embodiment 1, except that the raw material for preparing the ceramic reinforcing particles is clay.
The preparation method of the ceramic reinforced particle of the embodiment comprises the following steps: the clay was made into a spherical shape having a particle diameter of 1 to 3mm, and calcined at 900 ℃ for 8 hours to obtain ceramic reinforcing granules of this example.
Example 4
The double-layer high-strength heat-preservation refractory castable and the preparation method thereof are the same as those in example 1, except that the mass ratio of the silica-alumina sol to the clay is 0.2: 1.
Example 5
The double-layer high-strength heat-preservation refractory castable and the preparation method thereof are the same as those in example 1, except that the mass ratio of the silica-alumina sol to the clay is 0.04: 1.
Example 6
The dual-layer high-strength heat-preservation refractory castable and the preparation method thereof in this embodiment are the same as those in embodiment 4, except that the composite microcapsule particles sequentially comprise an inorganic layer and an internal filler from outside to inside, and a curing agent is not added to the outer-layer castable.
The preparation method of the composite microcapsule particle of the present embodiment includes the following steps:
(1) mixing aluminum powder and calcium hydroxide powder with equal mass with the silicon-aluminum sol, and performing ultrasonic treatment to uniformly disperse the mixture to obtain second mixed slurry;
(2) filtering the second mixed slurry and drying at 100 ℃ to obtain second powder;
(3) and roasting the second powder at 500 ℃ for 6 hours to obtain a prefabricated blank, soaking the prefabricated blank in water for 0.5 hour, and drying at 30 ℃ to obtain the composite microcapsule particles.
Example 7
The dual-layer high-strength heat-preservation refractory castable and the preparation method thereof in this embodiment are the same as those in embodiment 4, except that the composite microcapsule particles sequentially comprise an organic layer and an internal filler from outside to inside.
The preparation method of the composite microcapsule particle of the present embodiment includes the following steps:
(1) dissolving phenolic resin and aluminum ethoxide in ethanol according to the mass ratio of 1:0.02, and uniformly mixing to obtain a coating solution;
(2) mixing aluminum powder and calcium hydroxide powder with equal mass with the coating liquid, carrying out ultrasonic treatment for 20min, taking out the solid with the coating liquid on the surface, and drying at room temperature to remove ethanol to obtain the composite microcapsule particles with wet surfaces.
Example 8
The dual-layer high-strength heat-preservation refractory castable and the preparation method thereof in the embodiment are the same as those in the embodiment 4, and the difference is that the internal filler of the composite microcapsule particles is common sandy soil.
In the preparation method of the composite microcapsule particles of this example, ordinary sandy soil was used instead of the aluminum powder and the calcium hydroxide powder.
Example 9
The dual-layer high-strength heat-preservation refractory castable and the preparation method thereof in the embodiment are the same as those in the embodiment 4, and are different in that only aluminum powder is used as an internal filler of the composite microcapsule particles, only aluminum powder is used in the corresponding preparation method of the composite microcapsule particles, and the prefabricated blank can be directly added into the coating liquid without water immersion treatment.
Example 10
The dual-layer high-strength heat-preservation refractory castable and the preparation method thereof in this embodiment are the same as those in embodiment 4, except that the internal filler of the composite microcapsule particles is only calcium hydroxide, and only calcium hydroxide is used in the corresponding preparation method of the composite microcapsule particles.
Example 11
The dual-layer high-strength heat-preservation refractory castable and the preparation method thereof in the embodiment are the same as those in the embodiment 4, and the difference is that the aluminum powder and the calcium hydroxide are separately prepared into composite microcapsule particles, namely, some composite microcapsule particles only contain the aluminum powder, and some composite microcapsule particles only contain the calcium hydroxide.
The preparation method of the composite microcapsule particles comprises the following steps: (1) mixing aluminum powder and the silicon-aluminum sol, performing ultrasonic treatment to disperse uniformly to obtain a third mixed slurry, mixing calcium hydroxide powder and the silicon-aluminum sol, and performing ultrasonic treatment to disperse uniformly to obtain a fourth mixed slurry; wherein the aluminum powder and the calcium hydroxide powder have the same mass;
(2) filtering the third mixed slurry, and drying at the temperature of 100-120 ℃ to obtain third powder, and filtering the fourth mixed slurry, and drying at the temperature of 100-120 ℃ to obtain fourth powder;
(3) roasting the third powder and the fourth powder at 500 ℃ for 6 hours respectively to obtain a first blank and a second prefabricated blank, soaking the second prefabricated blank in water for 0.5 hour, and drying at 30 ℃ to obtain a second blank;
(4) dissolving phenolic resin and aluminum ethoxide in ethanol according to the mass ratio of 1:0.02, and uniformly mixing to obtain a coating solution;
(5) and immersing the first embryo body and the second embryo body with equal mass into the coating liquid, performing ultrasonic treatment for 20min, taking out the embryo body with the coating liquid on the surface, and drying at room temperature to remove ethanol to obtain the composite microcapsule particles with wet surfaces.
Example 12
The double-layer high-strength heat-preservation refractory castable and the preparation method thereof are the same as those in the embodiment 11, and the difference is that the mass ratio of the phenolic resin to the aluminum ethoxide is 1: 0.12.
Example 13
The double-layer high-strength heat-preservation refractory castable and the preparation method thereof in the embodiment are the same as those in the embodiment 11, and are different from the embodiment in that the mass ratio of the phenolic resin to the aluminum ethoxide is 1: 0.01.
Example 14
The double-layer high-strength heat-preservation refractory castable and the preparation method thereof in the embodiment are the same as those in the embodiment 12, and the difference is that the inner-layer castable comprises the following raw materials in parts by weight: 60 parts of high-aluminum aggregate, 25 parts of silicon carbide, 7 parts of fine alumina powder, 5 parts of silicon micropowder, 5 parts of white corundum powder, 18 parts of ceramic reinforcing particles, 3 parts of metal silicon powder, 3 parts of spherical asphalt, 3 parts of cement, 0.2 part of explosion-proof agent and 0.2 part of dispersing agent.
Example 15
The double-layer high-strength heat-preservation refractory castable and the preparation method thereof in the embodiment are the same as those in the embodiment 12, and the difference is that the outer-layer castable comprises the following raw materials in parts by weight: 66 parts of high-aluminum aggregate, 20 parts of silicon carbide, 7 parts of fine alumina powder, 5 parts of silicon micropowder, 5 parts of white corundum powder, 15 parts of composite microcapsule particles, 3 parts of metal silicon powder, 3 parts of spherical asphalt, 3 parts of cement, 0.2 part of explosion-proof agent and 0.2 part of dispersing agent.
The inner layer castable and the outer layer castable of the above examples and comparative examples were poured outside a blast furnace, cured by baking, and measured for the room-temperature flexural strength at 1450 ℃ for 3 hours, and the room-temperature compressive strength and the apparent porosity at 1450 ℃ for 3 hours, with the results shown in tables 1 and 2 below.
Table 1 comparison of strength of inner layer castable of example and comparative example 1
| Normal temperature bending strength/MPa | Normal temperature compressive strength/Mpa | |
| Example 1 | 12.38 | 110 |
| Example 2 | 11.66 | 103 |
| Example 3 | 11.85 | 105 |
| Example 4 | 12.41 | 113 |
| Example 5 | 12.02 | 107 |
| Example 14 | 12.39 | 112 |
| Comparative example 1 | 9.61 | 77 |
TABLE 2 comparison of the apparent porosity of the outer layer casting materials of the examples and comparative example 1
| Apparent porosity/% | Apparent porosity/% | ||
| Example 1 | 14.9 | Example 12 | 15.0 |
| Example 6 | 10.8 | Example 13 | 15.3 |
| Example 7 | 12.5 | Example 15 | 15.1 |
| Example 8 | 16.2 | Comparative example 1 | 10.7 |
| Example 9 | 16.1 |
TABLE 3 comparison of the room-temperature rupture strengths of the outer castable materials of the examples and the comparative examples
As can be seen from Table 1, the inner layer castable prepared by the invention has higher compressive strength and rupture strength, and can effectively cope with the high-temperature use environment of the blast furnace tapping channel.
As shown in Table 2, the composite microcapsule particles of example 8 had no internal filler, and example 9 had no calcium hydroxide, but had a large apparent porosity, and could not absorb excessive CO released by carbonization of the organic layer2And a small amount of fine cracks appear on the surface of the outer-layer castable. The apparent porosity of example 12 was comparable to that of example 4, but the apparent pore distribution was more uniform. Although the apparent porosity of example 13 was slightly increased, the apparent pore distribution was not uniform. As can be seen from tables 2 and 3, the outer layer castable prepared by the invention has high compressive strength and apparent porosity and good heat preservation performance.
Claims (9)
1. The double-layer high-strength heat-preservation refractory castable is characterized by comprising an inner-layer castable and an outer-layer castable, wherein the inner-layer castable is prepared from raw materials including a first aggregate and a blending material, and the first aggregate comprises a silicon-aluminum aggregate and ceramic reinforcing particles;
the preparation raw materials of the outer-layer castable comprise a second aggregate and a blending material, wherein the second aggregate comprises a silicon-aluminum aggregate and composite microcapsule particles;
the silicon-aluminum aggregate comprises high-aluminum aggregate, silicon carbide, fine alumina powder, silicon micro powder and white corundum powder; the admixture comprises metal silicon powder, spherical asphalt, cement, an explosion-proof agent and a dispersing agent.
2. The castable refractory of claim 1, wherein the ceramic reinforcing particles are prepared from raw materials including silica-alumina sol and clay, and the ceramic reinforcing particles have a particle size of 1-3 mm.
3. The castable refractory of claim 2, wherein the ceramic reinforcing particles have a silica-alumina sol to clay mass ratio of (0.05-0.2): 1.
4. The castable refractory according to claim 2, wherein the composite microcapsule particles are spherical, and the particle size of the composite microcapsule particles is 1-5 mm.
5. The castable refractory according to claim 4, wherein the composite microcapsule particles comprise an organic layer, an inorganic layer and an internal filler from outside to inside in sequence, the components of the organic layer comprise phenolic resin, a carbon forming agent and aluminum ethoxide, the components of the inorganic layer comprise silica-alumina sol, and the internal filler comprises aluminum powder and/or calcium hydroxide.
6. The castable refractory of claim 5, wherein the outer castable further comprises a curing agent comprising methylol urea and sodium carbonate for curing phenolic resin;
the carbon forming agent is pentaerythritol.
7. The castable refractory according to claim 1, wherein the high alumina aggregate of the inner castable has a particle size of 5-8mm, the silicon carbide has a particle size of 0.5-1mm, the SiC content in the silicon carbide is not less than 98%, the alumina fine powder has a particle size of 5-8 μm, and Al in the alumina fine powder2O3The content of the silicon dioxide is not less than 87 percent, the grain diameter of the silicon micro powder is 0.1-0.5 mu m, and SiO in the silicon micro powder2The content is not less than 95 percent, and the grain diameter of the white alundum powder is 5-10 mm;
the inner layer castable comprises the following raw materials in parts by weight: 50-60 parts of high-aluminum aggregate, 15-25 parts of silicon carbide, 5-7 parts of fine aluminum oxide powder, 3-5 parts of silicon micropowder, 3-5 parts of white corundum powder, 10-18 parts of ceramic reinforced particles, 2-3 parts of metal silicon powder, 2-3 parts of spherical asphalt, 2-3 parts of cement, 0.1-0.2 part of explosion-proof agent and 0.1-0.2 part of dispersing agent.
8. According to the rightThe refractory castable of claim 6, wherein the high alumina aggregate of the outer castable has a particle size of 8-10mm, the silicon carbide has a particle size of 1-2mm, the SiC content in the silicon carbide is not less than 98%, the alumina fine powder has a particle size of 8-15 μm, and the Al in the alumina fine powder2O3The content of the silicon dioxide is not less than 87 percent, the grain diameter of the silicon micro powder is 0.5 to 1.5 mu m, and SiO in the silicon micro powder2The content is not less than 95 percent, and the grain diameter of the white alundum powder is 5-15 mm;
the outer-layer castable comprises the following raw materials in parts by weight: 55-66 parts of high-aluminum aggregate, 10-20 parts of silicon carbide, 5-7 parts of fine aluminum oxide powder, 3-5 parts of silicon micropowder, 3-5 parts of white corundum powder, 10-15 parts of composite microcapsule particles, 2-3 parts of metal silicon powder, 2-3 parts of spherical asphalt, 2-3 parts of cement, 0.1-0.2 part of explosion-proof agent and 0.1-0.2 part of dispersing agent.
9. The method of producing a castable refractory according to any one of claims 6, 7 and 8, including a method of producing the ceramic reinforcing particles, a method of producing composite microcapsule particles, a method of producing an inner castable and a method of producing an outer castable;
the preparation method of the ceramic reinforced particle comprises the following steps:
(1) mixing the silicon-aluminum sol and the clay according to the mass ratio (0.05-0.2) to 1 to obtain first mixed slurry;
(2) filtering the first mixed slurry, and drying at the temperature of 100-120 ℃ to obtain first powder;
(3) roasting the first powder at the temperature of 900-1200 ℃ for 6-8h to obtain the ceramic reinforced particles;
the preparation method of the inner layer castable comprises the following steps:
(4) uniformly mixing the silicon-aluminum aggregate of the inner-layer castable and the ceramic reinforcing particles according to the mass parts to obtain inner-layer premix;
(5) mixing the inner-layer premix and the blended material according to the mass parts, and uniformly stirring to obtain an inner-layer castable;
the preparation method of the composite microcapsule particles comprises the following steps:
(6) mixing aluminum powder and calcium hydroxide powder with the silicon-aluminum sol, and performing ultrasonic treatment to disperse uniformly to obtain second mixed slurry;
(7) filtering the second mixed slurry and drying at the temperature of 100-120 ℃ to obtain second powder;
(8) roasting the second powder at the temperature of 500-700 ℃ for 5-6h to obtain a prefabricated blank, soaking the prefabricated blank in water for 0.5-1h, and then drying at the temperature of 30-50 ℃ to obtain a blank;
(9) dissolving phenolic resin and aluminum ethoxide in the mass ratio of 1 (0.02-0.12) in ethanol, and uniformly mixing to obtain a coating solution;
(10) immersing the embryo body obtained in the step (8) into the coating liquid, carrying out ultrasonic treatment for 10-20min, taking out the embryo body with the coating liquid on the surface, and drying at room temperature to remove ethanol to obtain the composite microcapsule particles with wet surfaces;
the preparation method of the outer-layer castable comprises the following steps:
(11) uniformly mixing silicon-aluminum aggregate of the outer-layer castable, adding the composite microcapsule particles, uniformly mixing, adding the curing agent, and uniformly mixing to obtain an outer-layer premix;
(12) and mixing the outer-layer premix and the blended material according to the mass parts, and uniformly stirring to obtain the outer-layer castable.
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