TWI421227B - 無水泥耐火物 - Google Patents
無水泥耐火物 Download PDFInfo
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- TWI421227B TWI421227B TW096123930A TW96123930A TWI421227B TW I421227 B TWI421227 B TW I421227B TW 096123930 A TW096123930 A TW 096123930A TW 96123930 A TW96123930 A TW 96123930A TW I421227 B TWI421227 B TW I421227B
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- 239000000203 mixture Substances 0.000 claims description 111
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 56
- 239000011230 binding agent Substances 0.000 claims description 49
- 229910052751 metal Inorganic materials 0.000 claims description 48
- 239000002184 metal Substances 0.000 claims description 48
- 239000004568 cement Substances 0.000 claims description 44
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 22
- 239000000463 material Substances 0.000 claims description 22
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 18
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 16
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 16
- 239000010455 vermiculite Substances 0.000 claims description 16
- 229910052902 vermiculite Inorganic materials 0.000 claims description 16
- 235000019354 vermiculite Nutrition 0.000 claims description 16
- 239000002245 particle Substances 0.000 claims description 13
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 12
- 229910052782 aluminium Inorganic materials 0.000 claims description 12
- 238000001035 drying Methods 0.000 claims description 12
- 229910052799 carbon Inorganic materials 0.000 claims description 10
- 239000000395 magnesium oxide Substances 0.000 claims description 10
- 239000006174 pH buffer Substances 0.000 claims description 10
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 8
- 229910052684 Cerium Inorganic materials 0.000 claims description 8
- 238000004519 manufacturing process Methods 0.000 claims description 7
- 238000000034 method Methods 0.000 claims description 7
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 6
- 239000000956 alloy Substances 0.000 claims description 6
- 229910045601 alloy Inorganic materials 0.000 claims description 6
- 229940043430 calcium compound Drugs 0.000 claims description 6
- 150000001674 calcium compounds Chemical class 0.000 claims description 6
- 239000003795 chemical substances by application Substances 0.000 claims description 6
- 229910052742 iron Inorganic materials 0.000 claims description 6
- 239000011777 magnesium Substances 0.000 claims description 6
- 229910052749 magnesium Inorganic materials 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 5
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims description 4
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 4
- 229910052849 andalusite Inorganic materials 0.000 claims description 4
- 229910052804 chromium Inorganic materials 0.000 claims description 4
- 239000011651 chromium Substances 0.000 claims description 4
- 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 claims description 4
- UNASZPQZIFZUSI-UHFFFAOYSA-N methylidyneniobium Chemical compound [Nb]#C UNASZPQZIFZUSI-UHFFFAOYSA-N 0.000 claims description 4
- 229910052863 mullite Inorganic materials 0.000 claims description 4
- 229910052726 zirconium Inorganic materials 0.000 claims description 4
- 229910052580 B4C Inorganic materials 0.000 claims description 3
- 239000000654 additive Substances 0.000 claims description 3
- 239000003963 antioxidant agent Substances 0.000 claims description 3
- INAHAJYZKVIDIZ-UHFFFAOYSA-N boron carbide Chemical compound B12B3B4C32B41 INAHAJYZKVIDIZ-UHFFFAOYSA-N 0.000 claims description 3
- 229910052758 niobium Inorganic materials 0.000 claims description 3
- 239000010955 niobium Substances 0.000 claims description 3
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 claims description 3
- 229910052797 bismuth Inorganic materials 0.000 claims description 2
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 claims description 2
- 150000001875 compounds Chemical class 0.000 claims description 2
- 239000006179 pH buffering agent Substances 0.000 claims description 2
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 claims 5
- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 claims 2
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 claims 2
- 230000003078 antioxidant effect Effects 0.000 claims 2
- 229910052707 ruthenium Inorganic materials 0.000 claims 2
- 239000007787 solid Substances 0.000 claims 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims 1
- -1 aluminum gold Chemical compound 0.000 claims 1
- 229910052791 calcium Inorganic materials 0.000 claims 1
- 239000011575 calcium Substances 0.000 claims 1
- 239000004615 ingredient Substances 0.000 claims 1
- 229910052712 strontium Inorganic materials 0.000 claims 1
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 claims 1
- 239000000843 powder Substances 0.000 description 25
- 239000000126 substance Substances 0.000 description 15
- 229910052739 hydrogen Inorganic materials 0.000 description 10
- 239000001257 hydrogen Substances 0.000 description 10
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 9
- 238000006243 chemical reaction Methods 0.000 description 7
- 230000009257 reactivity Effects 0.000 description 7
- 230000000704 physical effect Effects 0.000 description 6
- 239000000919 ceramic Substances 0.000 description 5
- 239000000499 gel Substances 0.000 description 5
- 150000002739 metals Chemical class 0.000 description 5
- 238000009825 accumulation Methods 0.000 description 4
- 239000010426 asphalt Substances 0.000 description 4
- 239000000872 buffer Substances 0.000 description 4
- XFWJKVMFIVXPKK-UHFFFAOYSA-N calcium;oxido(oxo)alumane Chemical compound [Ca+2].[O-][Al]=O.[O-][Al]=O XFWJKVMFIVXPKK-UHFFFAOYSA-N 0.000 description 4
- 238000010304 firing Methods 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 4
- 239000002893 slag Substances 0.000 description 4
- 239000000853 adhesive Substances 0.000 description 3
- 230000001070 adhesive effect Effects 0.000 description 3
- ZMIGMASIKSOYAM-UHFFFAOYSA-N cerium Chemical compound [Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce] ZMIGMASIKSOYAM-UHFFFAOYSA-N 0.000 description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
- 238000004880 explosion Methods 0.000 description 3
- 239000000835 fiber Substances 0.000 description 3
- NFFIWVVINABMKP-UHFFFAOYSA-N methylidynetantalum Chemical compound [Ta]#C NFFIWVVINABMKP-UHFFFAOYSA-N 0.000 description 3
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 3
- 239000011148 porous material Substances 0.000 description 3
- 229910003468 tantalcarbide Inorganic materials 0.000 description 3
- 230000002411 adverse Effects 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000007767 bonding agent Substances 0.000 description 2
- 239000011449 brick Substances 0.000 description 2
- 239000006172 buffering agent Substances 0.000 description 2
- 238000005266 casting Methods 0.000 description 2
- 239000004927 clay Substances 0.000 description 2
- 239000012141 concentrate Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000009970 fire resistant effect Effects 0.000 description 2
- HYBBIBNJHNGZAN-UHFFFAOYSA-N furfural Chemical compound O=CC1=CC=CO1 HYBBIBNJHNGZAN-UHFFFAOYSA-N 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 238000002309 gasification Methods 0.000 description 2
- 150000002431 hydrogen Chemical class 0.000 description 2
- 238000006460 hydrolysis reaction Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 2
- 238000011065 in-situ storage Methods 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 239000011819 refractory material Substances 0.000 description 2
- 239000011029 spinel Substances 0.000 description 2
- 229910052596 spinel Inorganic materials 0.000 description 2
- 229910000838 Al alloy Inorganic materials 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 238000004026 adhesive bonding Methods 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 150000001340 alkali metals Chemical class 0.000 description 1
- INJRKJPEYSAMPD-UHFFFAOYSA-N aluminum;silicic acid;hydrate Chemical compound O.[Al].[Al].O[Si](O)(O)O INJRKJPEYSAMPD-UHFFFAOYSA-N 0.000 description 1
- 229910052787 antimony Inorganic materials 0.000 description 1
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 description 1
- 238000010420 art technique Methods 0.000 description 1
- 239000010953 base metal Substances 0.000 description 1
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 1
- 239000004327 boric acid Substances 0.000 description 1
- 239000006229 carbon black Substances 0.000 description 1
- 239000002738 chelating agent Substances 0.000 description 1
- 238000004939 coking Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 239000004567 concrete Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000001066 destructive effect Effects 0.000 description 1
- 239000002612 dispersion medium Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000010459 dolomite Substances 0.000 description 1
- 229910000514 dolomite Inorganic materials 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 229910052839 forsterite Inorganic materials 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 239000010443 kyanite Substances 0.000 description 1
- 229910052850 kyanite Inorganic materials 0.000 description 1
- 229910001338 liquidmetal Inorganic materials 0.000 description 1
- 239000001095 magnesium carbonate Substances 0.000 description 1
- 229910000021 magnesium carbonate Inorganic materials 0.000 description 1
- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 description 1
- 235000014380 magnesium carbonate Nutrition 0.000 description 1
- HCWCAKKEBCNQJP-UHFFFAOYSA-N magnesium orthosilicate Chemical compound [Mg+2].[Mg+2].[O-][Si]([O-])([O-])[O-] HCWCAKKEBCNQJP-UHFFFAOYSA-N 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 235000010755 mineral Nutrition 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 229910052609 olivine Inorganic materials 0.000 description 1
- 239000010450 olivine Substances 0.000 description 1
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- 239000005011 phenolic resin Substances 0.000 description 1
- 229920001568 phenolic resin Polymers 0.000 description 1
- 150000002989 phenols Chemical class 0.000 description 1
- 235000021317 phosphate Nutrition 0.000 description 1
- 150000003013 phosphoric acid derivatives Chemical class 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 230000002028 premature Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000011214 refractory ceramic Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 150000004760 silicates Chemical class 0.000 description 1
- 239000011041 smoky quartz Substances 0.000 description 1
- 239000001509 sodium citrate Substances 0.000 description 1
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
- 229910001928 zirconium oxide Inorganic materials 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C29/00—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides
- C22C29/005—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides comprising a particular metallic binder
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C29/00—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides
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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
- C04B35/10—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on aluminium oxide
- C04B35/101—Refractories from grain sized mixtures
- C04B35/103—Refractories from grain sized mixtures containing non-oxide refractory materials, e.g. carbon
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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
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/62605—Treating the starting powders individually or as mixtures
- C04B35/62625—Wet mixtures
- C04B35/6263—Wet mixtures characterised by their solids loadings, i.e. the percentage of solids
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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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- 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
- C04B2235/3206—Magnesium oxides or oxide-forming salts thereof
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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
- C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
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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
- C04B2235/32—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
- C04B2235/3222—Aluminates other than alumino-silicates, e.g. spinel (MgAl2O4)
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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
- C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
- C04B2235/3244—Zirconium oxides, zirconates, hafnium oxides, hafnates, or oxide-forming salts thereof
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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
- C04B2235/34—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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- C04B2235/00—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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Description
本發明係有關一種耐火混合物。混合物含有pH緩衝劑及煙燻矽石或矽金屬。混合物可藉習知技術形成來形成耐火物件。耐火物件具有比較含有基於水泥之黏結劑及化學黏結劑之材料更優異的物理性質,包括耐火性質更高。
耐火物件包括預成形產物及原位成形產物。預成形產物包括罩蓋、管子、板子及磚塊。成形產物可用作為容器、管子或通道的內襯,成形產物經常係以混合物形式提供而可於現場注塞、槍射擊、鏝塗、噴霧、振搖或澆鑄。
耐火物件必須可對抗熱攻擊、化學攻擊及機械攻擊。熱攻擊包括高溫,經常係高於1000℃,熱衝擊係由物件溫度的快速改變所造成。經常耐火物件的應用用途係用來包括或產生破壞化學品。例如存在於剛澆鑄中的熔渣會化學攻擊耐火物件,故於熔渣接觸的物件經常必須為耐熔渣的氧化物諸如氧化鋯。同理,用於鋁淨靜鋼的耐火管必須可對抗氧化鋁的堆積,否則氧化鋁的堆積將造成管子的阻塞。最後,耐火物件須夠強來對抗機械力諸如壓縮應力、拉力及扭變應力。
常見耐火物件係由耐火聚積體與黏結劑的組合所形成。黏結劑將聚積體固定定位。聚積體和黏結劑顯著影響物件的性質。常見聚積體包括矽石、氧化鋯、碳化矽、氧化鋁、氧化鎂、尖晶石、煅燒白雲石、鉻菱鎂礦、橄欖石、鎂橄欖石、富鋁紅柱石、藍晶石、紅柱石、燒黏土、碳、鉻鐵礦及其組合。
黏結劑分成兩大類,亦即水泥類及「化學類」。化學黏結劑包括有機化學品及無機化學品諸如酚類、糠醛、有機樹脂、磷酸鹽類及矽酸鹽類。物件常係經燒製來活化化學品,以及引發黏結劑。水泥黏結劑包括水泥或其它可水合之陶瓷粉末,諸如鋁酸鈣水泥或可水合之氧化鋁。經常無需加熱來活化黏結劑,但確實需要加水。水與水泥黏結劑反應來硬化混合物。水也用作為細小粉末的分散介質。乾粉之流動性不佳,亦不適合用於無高壓存在下形成耐火物件。水降低混合物黏度,藉此允許聚積體/黏結劑混合物流動。不幸於耐火物件中存在有水具有嚴重影響,也就是當物件暴露於高溫時造成物件裂開,甚至於耐火溫度時出現爆炸氣化現象。含水泥黏結劑之物件經常需要乾燥步驟來去除殘餘之水。
耐火聚積體/黏結劑混合物典型包含至少70 wt.%聚積體及至多約15 wt.%水泥黏結劑。加水來組成混合物之差額,水量係足夠產生形成耐火物件期望的流動性。水可直接添加或以水合物形式添加。例如,歐洲專利申請公告案第0064863號以無機水合物形式加水,該無機水合物可於升高溫度時分解。US 6,284,688於微包囊之矽酸鈉中包括水。
物件之孔隙度影響乾燥速率和爆炸氣化風險,原因在於孔隙允許水由物件中蒸發或氣化。先前技術藉加入金屬粉末來提高混合物之孔隙度。JP 38154/1986之教示包含聚積體、水泥及鋁粉的耐火混合物。鋁粉與所添加之水反應,製造氫氣。氣泡狀的氣體形成孔隙,通過該等孔隙可乾燥並釋放出水蒸氣。鋁反應產生大量熱,大量熱量進一步有助於乾燥。使用鋁粉的問題包括強放熱反應、釋放出可燃性氫氣、於物件中形成微裂縫、及鋁粉的儲存壽命有限。為了控制此種反應性,US 5,783,510及US 6,117,373教示一種包含耐火聚積體、耐火粉末及反應性金屬粉末之單晶耐火組成物。耐火粉末包括含鋁水泥來黏合聚積體,藉此對藉該組成物所形成的物件提供物理強度。反應性金屬包括鋁、鎂、矽及其合金。反應性金屬含量經選定來控制氫氣的產生,藉此控制孔隙度。另外,日本專利公開案第190276/1984號教示使用纖維來形成細小通道,水可通過該等通道而逃逸。不幸,纖維難以均勻分散於混合物內,且纖維造成流動性的降低。物件的孔隙度也增高,對物件成品的物理性質造成不良影響。
耐火物件包括可免除水的需要之化學黏結劑,換言之非水泥黏結劑。黏度典型極高,聚積體/化學黏結劑混合物經常無法良好流動。化學黏結劑典型係藉於升高溫度加熱或燒製來活化,例如係用於可乾燥振搖混合物內及多種預成形物件中。US 6,846,763包含粒化瀝青作為黏結劑,以及含有耐火聚積體、可燃性金屬粉末及油。加熱混合物將金屬粉末點燃,金屬粉末燃燒油,而造成瀝青的熔解與焦化。結果為經碳鍵結的耐火物件。典型組成物包括70 wt.%聚積體、6 wt.%矽、7 wt.%油及13 wt.%瀝青。雖然要求高溫來形成碳鍵,但該物件實質上不含水。碳鍵結物件不如氧化物鍵結物件的安定。除非維持於還原氣氛下,否則碳鍵結物件也對於升高溫度下的氧化敏感。
US 5,366,944教示使用低溫黏結劑及高溫黏結劑之一種耐火組成物。未添加水至該組成物。低溫黏結劑包括有機黏結劑,例如酚系樹脂。高溫黏結劑包括鋁、矽、鎂、及其合金及混合物之金屬粉末。可由該組成物形成物件,於低溫固化來活化低溫黏結劑。低溫黏結劑將物件結合在一起,直到物件被安裝,高溫黏結劑活化為止。直至達耐火溫度前,金屬黏結劑不會被活化。另外,金屬黏結劑製造具有比基於水泥之黏結劑更高耐火性質之物件。
具有低水含量及低孔隙度之非基於水泥之耐火混合物來製造於高溫具有高強度的耐火物件有其需求存在。
本發明係有關一種可獲得耐火組成物之混合物,該混合物例如可用作為各種冶金容器的內襯,諸如熔爐、盛桶、漏斗及坩堝之內襯。組成物也可全部或部分用於導引液體金屬流動之物件。混合物需要比傳統基於水泥之系統更少量水,藉此來縮短乾燥時間及降低爆炸的風險。混合物無需燒製來達成初步硬化。較佳混合物比較基於水泥之混合物也可提高所得物件的耐火性及強度。
就廣義態樣而言,本發明為包括耐火聚積體與可製造pH緩衝劑之物質的無水泥混合物。該混合物含有含細粉狀金屬成分之黏結劑。該應用用途指示原料,諸如耐火聚積體及黏結劑之化學組成及粒徑的選擇及分。相信有大表面積的聚積體成分諸如煙燻矽石可製造凝膠,凝膠作用來形成有低水含量及低水孔隙度之耐火材料。須瞭解此處述及煙燻矽石用作為聚積體成分係有關無水煙燻矽石,與膠體矽石區別。相信存在有可製造pH緩衝劑之物質諸如氧化鎂、氧化鋁、氧化鋯或非水泥鈣化合物或此等材料的組合也可用來形成具有低水含量及低水孔隙度之耐火材料。
本發明之混合物需要比傳統基於水泥之混合物更少量水。此外添加定量之水至該聚積體/黏結劑混合物,導致比基於水泥之混合物更高的流動性。物件之物理性質也比較基於水泥之物件,對添加水量之相依性較低。
於一個實施例中,混合物包含耐火聚積體及0.5wt.%至5wt.%具有粒徑為-200網目或更細小的金屬粉末。依據用途而定,添加足量水至該混合物。混合物之pH經調整而防止或減少氫氣的逸出至可接受的低程度。如熟諳技藝人士已知,可使用緩衝劑來維持pH。視情況需要,可添加去絮凝劑來改良流動特性或降低水量需求。然後將聚積體/黏結劑/水摻合物成形為任何期望的形狀。該成形體硬化而形成物件。於窯中加熱或於使用溫度加熱,製造氧化物鍵結物件。
黏結劑的較佳用途係用於可澆鑄之耐火配方。黏結劑也可用於其它類型的耐火物件,例如塑膠材料、注塞材料、磚塊及壓製成形件。熟諳技藝人士瞭解需要調整儲存壽命及形成順序,來於適當時間間隔達成鍵結的硬化固定。
於特定實施例中,包含燒製黏土聚積體及煙燻矽石之耐火聚積體與1wt.%鋁粉、0.5wt.%氧化鎂緩衝劑及0.2wt.%去絮凝劑組合。添加5wt.%水,成形為期望的形狀。控制pH,減少氫氣的逸出及降低所得孔隙度。燒製可製造具有較低孔隙度之緊密氧化物鍵結物件。
本發明之混合物含有聚積體及可獲得pH緩衝劑之物質。本發明之混合物可不使用水泥來獲得耐火組成物。根據本發明之無水泥混合物含有低於3.3 wt.%此處呈現之比較例之水泥含量,及含有低於0.2 wt.%水泥。
黏結劑可與陶瓷聚積體特別為耐火陶瓷聚積體組合用於本發明。黏結劑不含水泥,並可實質上由金屬粉末組成。形成包含聚積體、金屬粉末黏結劑及pH緩衝劑之混合物。添加足量水至該混合物。然後含水混合物形成為物件。不似基於水泥之黏結劑,本黏結劑具有類似或大於聚積體之耐火程度。使用金屬黏結劑所製造之物件之物理性質也能超過使用傳統黏結劑系統所製造之物件之物理性質。
本發明非僅限於任何特定陶瓷聚積體,換言之,陶瓷聚積體可具有任何適當之化學組成或粒徑、形狀或分佈。常見聚積體包括矽石、氧化鋯、碳化矽、氧化鋁、氧化鎂、尖晶石及其組合。聚積體可包括煙燻材料。於本發明之一個實施例中,聚積體含有煙燻矽石及物質,諸如氧化鋁、氧化鎂、氧化鋯或非水泥鈣化合物或此等材料之組合來獲得pH緩衝劑。使用耐火物件之用途大為決定耐火聚積體的組成。鍵結同樣也適合製造用於非耐火用途之可澆鑄物。適當金屬及聚積體可用來製造可用於周圍溫度結構之可澆鑄物。典型用途為土木工程(橋樑、建築物、道路等)、特用混凝土及修補材料。
黏結劑可實質上係由金屬粉末所組成,不含水泥諸如鋁酸鈣水泥,黏結劑典型具有比陶瓷聚積體更低的強度和更低的耐火度。金屬粉末包括任何可與水反應來形成聚積體粒子間之錯合物之金屬。錯合物例如可為氫氧化物凝膠。金屬粉末之反應性不可過高,而造成與水之反應速率無法控制。反應性係至少依據容器之pH、所使用之金屬、以及金屬的尺寸及形狀決定。例如鹼金屬與水激烈反應,而與pH無關。金屬粉末不可太過惰性,結果造成鍵結的硬化固定時間過長或不存在。非反應性金屬包括貴金屬及其它具有低化學電位之過渡金屬。
適當黏結劑用之金屬包括但非限於鋁、鎂、矽、鐵、鉻、鋯、其合金及其混合物。此等金屬之反應性可藉調整各項因素包括pH及金屬粉末之粒徑加以控制。與水混合後形成凝膠,凝膠黏結物件直到於升溫,形成氧化物鍵結而將聚積體黏結在一起。氧化物鍵結比鋁酸鈣水泥及多種其它黏合技術的耐火性更高。
聚積體/黏結劑/水混合物之pH須控制成讓氫氣的逸出係維持於可接受的限度以內。氫氣的產生可能為劇烈且爆炸性放熱。氫氣逸出的額外不利影響包括孔隙度增高及氫氧化物凝膠錯合物的過早分解。控制氫氣逸出所需的pH將依據所使用之金屬決定。此種pH可經計算,且係基於金屬之化學電位決定。可選用可維持pH之聚積體。另外,需要緩衝劑來維持期望的pH。適當緩衝劑為熟諳技藝人士所已知,包括氧化鎂、氧化鋁、氧化鋯及非水泥鈣化合物及此等物質的組合。較佳緩衝劑本身為耐火性,或緩衝劑將於使用溫度分解氣化。可添加螯合劑諸如檸檬酸或硼酸來控制固定硬化時間。本發明可以pH不大於10.0之混合物實施。
金屬/水反應之動力學也係藉金屬粉末之粒徑控制。金屬粉末之反應性係與可利用的表面積成正比。表面積愈大所得反應性愈高。金屬粉末之有效粒徑為-70網目(212微米)或更小。粒徑過大,限制反應性,粒徑過小則將造成反應動力學難以控制。方便的粒徑大小為-200網目(75微米)至-325網目(45微米)。粒徑只是控制表面積中之一個手段。也須改變金屬粉末之形狀或質地。另外,金屬粉末表面可以鈍化劑塗覆諸如為聚合物、蠟或氧化物。
金屬黏結劑之含量隨期望之應用用途、耐火聚積體、金屬及期望之固定硬化速度等而改變。黏結劑典型含量係於占混合物由0.5 wt.%至5 wt.%之範圍。低抵0.1 wt.%為有效,高達10 wt.%為合乎期望。更低量黏結劑可降低固定硬化速度及物件成品的強度。足量黏結劑含括於混合物來達成期望的性質。黏結劑含量較高將提高成本與提高自生反應的風險。對鋁金屬而言,約1 wt.%濃度可滿意地用於可澆鑄用途。若使用某些聚積體成分,諸如煙燻矽石,則可不使用金屬黏結劑來製造本發明之混合物。特別,根據本發明之混合物可不使用鋁合金粉末而製備。
視情況需要,可含括多種添加劑來改良物件製備期間或物件製備後之物理性質。可添加去絮凝劑來改良流動性及降低水的需求。碳例如呈碳黑或瀝青可添加至其中來對抗使用期間的熔渣穿透。諸如碳化硼或矽等抗氧化劑可保護碳避免氧化。其它添加劑為熟諳技藝人士眾所周知。
製造兩種可澆鑄聚積體/黏結劑混合物。兩種混合物意圖用作為高爐鐵斜槽和鐵澆道之耐火內襯。第一混合物為典型之可澆鑄「超低」水泥包含74 wt.%氧化鋁、17.5 wt.%碳化矽、3.3 wt.%鋁酸鈣水泥、2.5 wt.%煙燻矽石、及0.2 wt.%金屬粉末。第二混合物為本發明之無水泥組成物包含69 wt.%氧化鋁、22.5 wt.%碳化矽、6wt.%煙燻矽石、0.75 wt.%矽及0.5 wt.%鋁。
加水至兩種混合物。基於水泥之混合物要求4.25%-6.25 wt.%水來獲得ASTMC-1445流動性20%-100%。無水泥混合物只需要2.75-3.75 wt.%水來獲得20%-100%流動性。無水泥組成物只需要約半量水來達成期望的流動性。
允許混合物及水固定硬化。於固定硬化期間,第一混合物中之水泥將pH升高至超過10.0,因而有利於鋁粉與水間的水解反應。反應產生氫氣及熱。氫氣由混合物中除氣,而產生孔隙及空隙。熱可加速乾燥時間。相反地,第二混合物之pH維持低於10.0,部分原因係在於不存在有水泥之故。藉此水解係以氣體排出來作檢查。無水泥混合物之密度係高於基於水泥之混合物。乾燥後超低水泥混合物之孔隙度係由16%變化至24%。無水泥混合物之孔隙度為13-15%。
於用來移除任何殘水之前,超低水泥混合物及無水泥混合物須經乾燥。較佳,如前文說明,無水泥物件所需水量係顯著低於基於水泥之混合物,因而可加速乾燥。一旦乾燥且調整至超過800℃之使用溫度,則無水泥材料顯示比超低水泥材料更高的斷裂熱模量(HMOR)。HMOR係根據ASTM C-583施行。無水泥可澆鑄物之HMOR於800、1100、1370及1480℉分別為10.3、20.7、8.6及2.8 MPa。超低水泥可澆鑄物於每個溫度有較低HMOR,換言之於800、1100、1370及1480℃分別為6.2、4.8、5.5及2.1 MPa。
雖然已經就特定實施例說明本發明,但熟諳技藝人士顯然易知多種其它變化及修改及其它用途。本發明並非受此處之特定揭示所限。
Claims (36)
- 一種用於製造耐火物件之耐火混合物,其特徵為不存在有水泥,係包含:a)pH緩衝劑;以及b)包含煙燻矽石及/或金屬黏結劑之耐火聚積體。
- 如申請專利範圍第1項之耐火混合物,其特徵在於該pH緩衝劑包含氧化鋯、氧化鋁、氧化鎂、或非水泥鈣化合物或其組合。
- 如申請專利範圍第1項或第2項之耐火混合物,其特徵在於該混合物包括具有粒徑不大於70網目之金屬的黏結劑。
- 如申請專利範圍第3項之耐火混合物,其特徵在於存在有至少65wt.%耐火聚積體及0.1-10wt.%金屬。
- 如申請專利範圍第1項之耐火混合物,其特徵在於該金屬包含鋁、矽、鎂、鉻、鋯或鐵或其組合或其合金。
- 如申請專利範圍第1項之耐火混合物,其特徵在於該金屬包含矽。
- 如申請專利範圍第1項之耐火混合物,其特徵在於當與水混合來形成具有期望之流動性之混合物時,具有pH不大於10.0。
- 一種由如申請專利範圍第1項之耐火混合物所形成之耐火物件,其特徵在於該耐火物件係由下述方式製得:a)混合耐火聚積體與pH緩衝劑;b)添加足量水來形成具有期望之流動性及pH之混合物; c)將該混合物形成為一物件;d)允許該物件固定硬化;以及e)乾燥該成形件來去除過量水。
- 如申請專利範圍第8項之耐火物件,其特徵在於於乾燥後加熱該物件至使用溫度。
- 如申請專利範圍第8項或第9項之耐火物件,其特徵在於該pH緩衝劑為氧化鋯、氧化鋁、氧化鎂、或非水泥鈣化合物或其組合。
- 如申請專利範圍第8項之耐火物件,其特徵在於將該耐火聚積體與一種包含具有粒徑不大於70網目之金屬的黏結劑混合。
- 如申請專利範圍第8項之耐火物件,其特徵在於該金屬為鋁、矽、鎂、鉻、鋯或鐵或其組合或其合金。
- 如申請專利範圍第8項之耐火物件,其特徵在於該金屬為矽。
- 如申請專利範圍第8項之耐火物件,其特徵在於該pH係不大於10.0。
- 一種製造如申請專利範圍第1項之耐火物件之方法,其特徵在於:a)混合耐火聚積體與pH緩衝劑;b)添加足量水來形成具有期望之流動性之混合物;c)將該混合物形成為一物件;d)允許該物件固定硬化;以及e)乾燥該成形件來去除過量水。
- 如申請專利範圍第15項之方法,其特徵在於該pH緩衝 劑包含氧化鋯、氧化鋁、氧化鎂、或非水泥鈣化合物或其組合。
- 如申請專利範圍第15項或第16項之方法,其特徵在於將該耐火聚積體與一種包含具有粒徑不大於70網目之金屬的黏結劑混合。
- 如申請專利範圍第15項之方法,其特徵在於該金屬包含鋁、矽、鎂、鉻、鋯或鐵或其組合或其合金。
- 如申請專利範圍第15項之方法,其特徵在於該金屬包含矽。
- 如申請專利範圍第15項之方法,其特徵在於該pH係不大於10.0。
- 一種用於製造耐火物件之耐火混合物,包含:a)一種選自氧化鋁、紅柱石、富鋁紅柱石、及此些材料的組合之物質;b)碳化矽;c)煙燻矽石;d)鋁金屬;e)抗氧化劑,其係選自碳化硼、矽及此些材料之組合;f)反應性氧化鋁;以及g)碳。
- 如申請專利範圍第21項之耐火混合物,包含:a)至少69重量%且至多74重量%的一種選自氧化鋁、紅柱石、富鋁紅柱石、及此些材料的組合之物質;b)至少17.5重量%且至多22.5重量%的碳化矽;c)至少2.5重量%且至多6重量%的煙燻矽石; d)至少0.2重量%且至多1重量%的鋁金屬;e)至少0.75重量%且至多6重量%的矽;f)反應性氧化鋁;以及g)碳。
- 如申請專利範圍第21項之耐火混合物,其中含鈣化合物之量低於3.3重量%。
- 如申請專利範圍第21項之耐火混合物,進一步包含一種選自氧化鋯及氧化鎂之群組的材料。
- 如申請專利範圍第21項之耐火混合物,其中煙燻矽石具有不大於70網目之粒徑。
- 如申請專利範圍第21項之耐火混合物,進一步包含去絮凝劑。
- 如申請專利範圍第21項之耐火混合物,其中存在的鋁及矽組合含量係在自包含0.2重量%至包含5重量%之範圍內。
- 如申請專利範圍第21項之耐火混合物,其中存在的鋁及矽組合含量係在自包含0.5重量%至包含5重量%之範圍內。
- 如申請專利範圍第21項之耐火混合物,其中存在的碳化矽含量係在自包含17.5重量%至包含22.5重量%之範圍內。
- 如申請專利範圍第21項之耐火混合物,其中存在的煙燻矽石含量係在自包含2.5重量%至包含6重量%之範圍內。
- 如申請專利範圍第21項之耐火混合物,其中存在的鋁金 屬含量係在自包含0.5重量%至包含1重量%之範圍內。
- 如申請專利範圍第21項之耐火混合物,其中水泥之含量等於或低於0.2重量%。
- 如申請專利範圍第21項之耐火混合物,實質上由下列所組成:a)一種選自氧化鋁、紅柱石、富鋁紅柱石、及此些材料的組合之物質;b)碳化矽;c)煙燻矽石;d)鋁金屬;e)抗氧化劑,其係選自碳化硼、矽及此些材料之組合;f)反應性氧化鋁;g)碳;以及h)添加劑。
- 一種由如申請專利範圍第21項之耐火混合物所形成之耐火物件,該耐火物件係由具下述特徵之方法製得:a)混合固體成分;b)添加足量水來形成具有期望之流動性及pH之混合物;c)將該混合物形成為一物件;d)允許該物件固定硬化;以及e)乾燥該成形件來去除過量水。
- 如申請專利範圍第34項之耐火物件,其特徵在於於乾燥後加熱該物件至使用溫度。
- 一種製造如申請專利範圍第21項之耐火物件之方法,其特徵在於: a)混合固體成分;b)添加足量水來形成具有期望之流動性之混合物;c)將該混合物形成為一物件;d)允許該物件固定硬化;以及e)乾燥該成形件來去除過量水。
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DE202013011886U1 (de) * | 2013-06-28 | 2014-09-03 | Refratechnik Holding Gmbh | Feuerfestes Erzeugnis |
CN107188583B (zh) * | 2017-07-12 | 2020-09-15 | 瑞泰科技股份有限公司 | 一种用于cfb锅炉内衬裂缝的填缝料 |
CN112851306A (zh) * | 2021-01-13 | 2021-05-28 | 湖南湘钢瑞泰科技有限公司 | 一种rh用快速烧结喷补料及其制备方法 |
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- 2007-07-06 MX MX2009000161A patent/MX2009000161A/es active IP Right Grant
- 2007-07-06 EA EA200900148A patent/EA013714B1/ru not_active IP Right Cessation
- 2007-07-06 CN CN2007800289471A patent/CN101501231B/zh not_active Expired - Fee Related
- 2007-07-06 CA CA2656695A patent/CA2656695C/en not_active Expired - Fee Related
- 2007-07-06 WO PCT/US2007/072927 patent/WO2008006053A2/en active Application Filing
- 2007-07-06 EP EP07812673A patent/EP2041329A2/en not_active Withdrawn
- 2007-07-06 AU AU2007269073A patent/AU2007269073B2/en not_active Ceased
- 2007-07-06 UA UAA200815195A patent/UA95290C2/uk unknown
- 2007-07-06 KR KR1020097002534A patent/KR20090031447A/ko active Search and Examination
- 2007-07-06 US US12/307,627 patent/US20100009840A1/en not_active Abandoned
- 2007-07-06 BR BRPI0714034A patent/BRPI0714034A8/pt not_active IP Right Cessation
-
2014
- 2014-09-19 JP JP2014191348A patent/JP2015044734A/ja active Pending
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Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
TW466219B (en) * | 1997-01-08 | 2001-12-01 | Taiko Refractories | Casting refractory composition and method of wet spraying thereof |
WO1999008804A1 (en) * | 1997-08-13 | 1999-02-25 | North American Refractories Co. | Cement-free refractory castable system for wet process pumping/spraying |
TW200502193A (en) * | 2003-05-14 | 2005-01-16 | Asahi Glass Ceramics Co Ltd | Zirconia based monothilic refractory |
Also Published As
Publication number | Publication date |
---|---|
CN101501231A (zh) | 2009-08-05 |
BRPI0714034A8 (pt) | 2018-01-02 |
WO2008006053A2 (en) | 2008-01-10 |
JP2010501449A (ja) | 2010-01-21 |
AR098449A2 (es) | 2016-05-26 |
MX2009000161A (es) | 2009-01-23 |
AU2007269073B2 (en) | 2013-02-28 |
JP2015044734A (ja) | 2015-03-12 |
CA2656695A1 (en) | 2008-01-10 |
TW200808678A (en) | 2008-02-16 |
AU2007269073A1 (en) | 2008-01-10 |
KR20090031447A (ko) | 2009-03-25 |
CN101501231B (zh) | 2012-10-03 |
EA200900148A1 (ru) | 2009-06-30 |
EP2041329A2 (en) | 2009-04-01 |
BRPI0714034A2 (pt) | 2012-12-04 |
AR061827A1 (es) | 2008-09-24 |
ZA200900040B (en) | 2010-05-26 |
EA013714B1 (ru) | 2010-06-30 |
CA2656695C (en) | 2016-04-12 |
JP5823666B2 (ja) | 2015-11-25 |
UA95290C2 (uk) | 2011-07-25 |
US20100009840A1 (en) | 2010-01-14 |
WO2008006053A3 (en) | 2008-03-27 |
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