DE102004026260A1 - New spinnable mass, obtained by reacting aluminum triacylate with carbonic acid and mixing with silicon dioxide containing solution, useful for preparing green fibers and/or ceramic fibers based on aluminum oxide - Google Patents
New spinnable mass, obtained by reacting aluminum triacylate with carbonic acid and mixing with silicon dioxide containing solution, useful for preparing green fibers and/or ceramic fibers based on aluminum oxide Download PDFInfo
- Publication number
- DE102004026260A1 DE102004026260A1 DE200410026260 DE102004026260A DE102004026260A1 DE 102004026260 A1 DE102004026260 A1 DE 102004026260A1 DE 200410026260 DE200410026260 DE 200410026260 DE 102004026260 A DE102004026260 A DE 102004026260A DE 102004026260 A1 DE102004026260 A1 DE 102004026260A1
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- Prior art keywords
- aluminum
- triacylate
- sio
- composition according
- spinnable
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- 229910052782 aluminium Inorganic materials 0.000 title claims abstract description 30
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title claims abstract description 28
- 239000000835 fiber Substances 0.000 title claims abstract description 26
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 18
- 239000000377 silicon dioxide Substances 0.000 title claims abstract description 9
- 239000000919 ceramic Substances 0.000 title claims abstract description 6
- 238000002156 mixing Methods 0.000 title claims abstract description 6
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 title abstract description 4
- 235000012239 silicon dioxide Nutrition 0.000 title abstract description 4
- BVKZGUZCCUSVTD-UHFFFAOYSA-N carbonic acid Chemical compound OC(O)=O BVKZGUZCCUSVTD-UHFFFAOYSA-N 0.000 title abstract 2
- ODIGIKRIUKFKHP-UHFFFAOYSA-N (n-propan-2-yloxycarbonylanilino) acetate Chemical group CC(C)OC(=O)N(OC(C)=O)C1=CC=CC=C1 ODIGIKRIUKFKHP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000000725 suspension Substances 0.000 claims abstract description 7
- 238000009987 spinning Methods 0.000 claims description 27
- 239000000203 mixture Substances 0.000 claims description 25
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 23
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 18
- -1 aluminum compound Chemical class 0.000 claims description 15
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 14
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims description 14
- 239000002253 acid Substances 0.000 claims description 12
- 150000001735 carboxylic acids Chemical class 0.000 claims description 12
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims description 8
- 238000000034 method Methods 0.000 claims description 8
- XBDQKXXYIPTUBI-UHFFFAOYSA-N dimethylselenoniopropionate Natural products CCC(O)=O XBDQKXXYIPTUBI-UHFFFAOYSA-N 0.000 claims description 7
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims description 7
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 6
- 238000004519 manufacturing process Methods 0.000 claims description 6
- 235000006408 oxalic acid Nutrition 0.000 claims description 6
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 6
- 150000007513 acids Chemical class 0.000 claims description 5
- 239000002904 solvent Substances 0.000 claims description 5
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 claims description 4
- 235000011054 acetic acid Nutrition 0.000 claims description 4
- 235000019253 formic acid Nutrition 0.000 claims description 4
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 claims description 3
- 235000019260 propionic acid Nutrition 0.000 claims description 3
- IUVKMZGDUIUOCP-BTNSXGMBSA-N quinbolone Chemical compound O([C@H]1CC[C@H]2[C@H]3[C@@H]([C@]4(C=CC(=O)C=C4CC3)C)CC[C@@]21C)C1=CCCC1 IUVKMZGDUIUOCP-BTNSXGMBSA-N 0.000 claims description 3
- 229910052710 silicon Inorganic materials 0.000 claims description 3
- 239000010703 silicon Substances 0.000 claims description 3
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 2
- 125000000468 ketone group Chemical group 0.000 claims description 2
- LCTONWCANYUPML-UHFFFAOYSA-N Pyruvic acid Chemical compound CC(=O)C(O)=O LCTONWCANYUPML-UHFFFAOYSA-N 0.000 claims 2
- 229940107700 pyruvic acid Drugs 0.000 claims 1
- HHUIAYDQMNHELC-UHFFFAOYSA-N [O-2].[O-2].[O-2].[Al+3].[Al+3].O=[Si]=O Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3].O=[Si]=O HHUIAYDQMNHELC-UHFFFAOYSA-N 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 24
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 9
- MJWPFSQVORELDX-UHFFFAOYSA-K aluminium formate Chemical compound [Al+3].[O-]C=O.[O-]C=O.[O-]C=O MJWPFSQVORELDX-UHFFFAOYSA-K 0.000 description 8
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 description 6
- 238000013459 approach Methods 0.000 description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 4
- 229960000583 acetic acid Drugs 0.000 description 4
- 238000000578 dry spinning Methods 0.000 description 4
- 239000011521 glass Substances 0.000 description 4
- 239000002244 precipitate Substances 0.000 description 4
- 239000002243 precursor Substances 0.000 description 4
- 238000010992 reflux Methods 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- 229940024548 aluminum oxide Drugs 0.000 description 3
- 150000007942 carboxylates Chemical class 0.000 description 3
- 150000001732 carboxylic acid derivatives Chemical class 0.000 description 3
- 239000007795 chemical reaction product Substances 0.000 description 3
- 239000004310 lactic acid Substances 0.000 description 3
- 235000014655 lactic acid Nutrition 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 229910002651 NO3 Inorganic materials 0.000 description 2
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 2
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 2
- 150000001242 acetic acid derivatives Chemical class 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical class [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 150000004675 formic acid derivatives Chemical class 0.000 description 2
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 2
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 2
- IDOWTHOLJBTAFI-UHFFFAOYSA-N phenmedipham Chemical compound COC(=O)NC1=CC=CC(OC(=O)NC=2C=C(C)C=CC=2)=C1 IDOWTHOLJBTAFI-UHFFFAOYSA-N 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 description 1
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- FERIUCNNQQJTOY-UHFFFAOYSA-M Butyrate Chemical compound CCCC([O-])=O FERIUCNNQQJTOY-UHFFFAOYSA-M 0.000 description 1
- FERIUCNNQQJTOY-UHFFFAOYSA-N Butyric acid Natural products CCCC(O)=O FERIUCNNQQJTOY-UHFFFAOYSA-N 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- BDAGIHXWWSANSR-UHFFFAOYSA-M Formate Chemical compound [O-]C=O BDAGIHXWWSANSR-UHFFFAOYSA-M 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- XBDQKXXYIPTUBI-UHFFFAOYSA-M Propionate Chemical compound CCC([O-])=O XBDQKXXYIPTUBI-UHFFFAOYSA-M 0.000 description 1
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 1
- DUQPQYXGMDGOJC-UHFFFAOYSA-K [Si](O)(O)(O)O.C(=O)[O-].[Al+3].C(=O)[O-].C(=O)[O-] Chemical compound [Si](O)(O)(O)O.C(=O)[O-].[Al+3].C(=O)[O-].C(=O)[O-] DUQPQYXGMDGOJC-UHFFFAOYSA-K 0.000 description 1
- ZMZINYUKVRMNTG-UHFFFAOYSA-N acetic acid;formic acid Chemical compound OC=O.CC(O)=O ZMZINYUKVRMNTG-UHFFFAOYSA-N 0.000 description 1
- 238000003915 air pollution Methods 0.000 description 1
- 230000001476 alcoholic effect Effects 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 238000005267 amalgamation Methods 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 150000004648 butanoic acid derivatives Chemical class 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- RCTYPNKXASFOBE-UHFFFAOYSA-M chloromercury Chemical compound [Hg]Cl RCTYPNKXASFOBE-UHFFFAOYSA-M 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 238000010411 cooking Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 239000013530 defoamer Substances 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- WCOATMADISNSBV-UHFFFAOYSA-K diacetyloxyalumanyl acetate Chemical class [Al+3].CC([O-])=O.CC([O-])=O.CC([O-])=O WCOATMADISNSBV-UHFFFAOYSA-K 0.000 description 1
- 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 description 1
- 238000001035 drying Methods 0.000 description 1
- 125000006575 electron-withdrawing group Chemical group 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000012362 glacial acetic acid Substances 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 150000002736 metal compounds Chemical class 0.000 description 1
- 229910052863 mullite Inorganic materials 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 150000007524 organic acids Chemical class 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 239000012266 salt solution Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000005201 scrubbing Methods 0.000 description 1
- 230000002269 spontaneous effect Effects 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- LFQCEHFDDXELDD-UHFFFAOYSA-N tetramethyl orthosilicate Chemical compound CO[Si](OC)(OC)OC LFQCEHFDDXELDD-UHFFFAOYSA-N 0.000 description 1
- ILJSQTXMGCGYMG-UHFFFAOYSA-N triacetic acid Chemical compound CC(=O)CC(=O)CC(O)=O ILJSQTXMGCGYMG-UHFFFAOYSA-N 0.000 description 1
- 231100000925 very toxic Toxicity 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
- 229910052727 yttrium Inorganic materials 0.000 description 1
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/62227—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products obtaining fibres
- C04B35/62231—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products obtaining fibres based on oxide ceramics
- C04B35/6224—Fibres based on silica
- C04B35/62245—Fibres based on silica rich in aluminium oxide
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/62227—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products obtaining fibres
- C04B35/62231—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products obtaining fibres based on oxide ceramics
- C04B35/62236—Fibres based on aluminium oxide
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- 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
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
- D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
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- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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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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- C04B2235/00—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
- C04B2235/3224—Rare earth oxide or oxide forming salts thereof, e.g. scandium oxide
- C04B2235/3225—Yttrium oxide 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
- C04B2235/32—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
- C04B2235/3409—Boron oxide, borates, boric acids, or oxide forming salts thereof, e.g. borax
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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
- C04B2235/44—Metal salt constituents or additives chosen for the nature of the anions, e.g. hydrides or acetylacetonate
- C04B2235/449—Organic acids, e.g. EDTA, citrate, acetate, oxalate
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Ceramic Engineering (AREA)
- Inorganic Chemistry (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Textile Engineering (AREA)
- Inorganic Fibers (AREA)
Abstract
Description
Die Erfindung betrifft die Synthese einer chlorid- und nitratfreien Spinnmasse zur Herstellung von Stapel- und anderen Fasern im System Al2O3-SiO2, insbesondere mit einem Aluminiumoxidgehalt höher als 60 %. Die neue Spinnmasse kann mit einer industriellen Zentrifugalspinnanlage zu Grünfasern versponnen und zum keramischen Endprodukt (Fasermatten oder dergleichen) verarbeitet werden.The invention relates to the synthesis of a chloride and nitrate-free spinning composition for the production of staple and other fibers in the system Al 2 O 3 -SiO 2 , in particular with an aluminum oxide content higher than 60%. The new dope can be spun with an industrial centrifugal spinning plant to green fibers and processed to the ceramic end product (fiber mats or the like).
Aus
der deutschen Patentschrift
In
der
Von Erfinderseite aus wurde der Versuch unternommen, das im genannten Patent vorgeschlagene Verfahren zu reproduzieren. So wurde Aluminiumformiat zunächst in heißem Wasser gelöst. Das frisch hydrolysierte Kieselsol wurde hergestellt, indem 200 g Kieselsäurester in Form von Tetramethoxysilan, 38 g Methanol, 0,4 ml 1n HCl, sowie 48 g Wasser unter Rühren vereinigt wurden. Nach weiterem halbstündigem Rühren war das SiO2-Sol gebrauchsfertig. Die dann vereinigte Aluminiumformiat-Kieselsäurelösung wurde bei 50°C und einem Druck von 20 mbar zu einem klaren Konzentrat mit einem Gesamtoxidgehalt von 12,5% Al2O3 und 0,25 SiO2 eingeengt. Durch Einrühren von 0,9% Polyethylenoxid (bezogen auf die Gesamtmasse der Lösung) mit einer mittleren Molekularmasse von 100.000 als Spinnhilfsmittel, das in wenig kaltem Methanol dispergiert war, wurde nach 15 stündigem langsamen Rühren und einer abschließenden Filtration eine Lösung erhalten, die zwar die geforderte Viskosität von 270 mPas aufwies, jedoch in Glasstabziehversuchen keinerlei Fäden bildete. Weiteres Einengen zur Verbesserung der Spinnbarkeit führte zu keinem Erfolg, da sich dabei ein weißer Niederschlag bildet.The inventors have made an attempt to reproduce the method proposed in said patent. For example, aluminum formate was first dissolved in hot water. The freshly hydrolyzed silica sol was prepared by combining 200 g of silicic acid ester in the form of tetramethoxysilane, 38 g of methanol, 0.4 ml of 1N HCl, and 48 g of water with stirring. After stirring for another half hour, the SiO 2 sol was ready for use. The then combined aluminum formate-silicic acid solution was concentrated at 50 ° C and a pressure of 20 mbar to a clear concentrate with a total oxide content of 12.5% Al 2 O 3 and 0.25 SiO 2 . By stirring 0.9% polyethylene oxide (based on the total mass of the solution) with a mean molecular weight of 100,000 as a spinning aid, which was dispersed in a little cold methanol, a solution was obtained after 15 hours of slow stirring and a final filtration, although the required viscosity of 270 mPas, but did not form any threads in Glasstabziehversuchen. Further concentration to improve the spinnability did not lead to success, as it forms a white precipitate.
In der Beschreibung dieses Patentes wird auch die Verwendung anderer Aluminiumcarboxylate vorgeschlagen. Demgemäß wird durch Auflösen von Aluminium oder Aluminiumhydroxid in einer einbasigen niedrigen Carbonsäure, wie z.B. Ameisensäure, Essigsäure, Propionsäure, vorzugsweise jedoch Ameisensäure, bei Temperaturen zwischen 40°C und 100°C eine Aluminiumsalzlösung erzeugt, wobei im allgemeinen 1,7, bis 3,2 Mole der organischen Säure auf 1 Mol angewandt werden, so dass in Lösung entweder basische oder neutrale Salze vorliegen. Dabei erhält man Homocarboxylate, die entweder Formiat, Acetat oder Propionat enthalten. Hieraus wird dann der Schluß gezogen, dass es auch ohne weiteres möglich sei, handelsübliche Aluminiumformiate oder Aluminiumacetate als Ausgangsmaterial heranzuziehen. Entsprechende Versuche der Erfinder führten jedoch nicht zum Erfolg.In The description of this patent will also make use of others Aluminum carboxylates proposed. Accordingly, by dissolving aluminum or aluminum hydroxide in a monobasic low carboxylic acid, such as e.g. Formic acid, acetic acid, propionic acid, preferably but formic acid, at temperatures between 40 ° C and 100 ° C an aluminum salt solution in general, 1.7 to 3.2 moles of organic Acid on 1 mol applied so that in solution either basic or neutral salts are present. This gives homocarboxylates, the contain either formate, acetate or propionate. This will become then the conclusion is drawn that it is also possible without further ado be, commercially available Use aluminum formates or aluminum acetates as starting material. However, corresponding attempts by the inventors did not lead to success.
Aluminiumhaltige Spinnmassen aus Cl-freien Vorstufen werden auch gemäß US-Patent 4954462 von Thomas Wood erhalten. Als Aluminiumquelle fungieren Aluminiumnitratformiatacetat oder basisches Aluminiumformiatacetat. Beim Einengen der Lösungen kommt es aufgrund der heterogenen Zusammensetzung mit zwei unterschiedlichen Carbonsäuren nicht zum Ausfallen eines Feststoffes, sondern zur Entstehung einer klaren viskosen Lösung. Durch Zugabe sehr geringer Mengen von Milchsäure (0,04 Mol, bezogen auf Al) wird das Fadenziehvermögen stark erhöht.aluminous Spun masses of Cl-free precursors are also disclosed in US Patent 4,954,462 received from Thomas Wood. The aluminum source is aluminum nitrate formate acetate or basic aluminum formate acetate. When concentrating the solutions comes it due to the heterogeneous composition with two different carboxylic acids not to the precipitation of a solid, but to the emergence of a clear viscous solution. By adding very small amounts of lactic acid (0.04 mol, based on Al) becomes the thread draw greatly increased.
Aluminiumnitratformiatacetat
kann aufgrund des Nitratgehaltes nicht als Ersatz für chlorhaltige Aluminiumverbindungen
in Betracht kommen. Eine Lösung
von basischem Aluminiumformiatacetat wird durch Umsetzung von Aluminium
mit einem Gemisch aus wässriger
Ameisen- und Essigsäure
hergestellt. Die Reaktionsdauer ist enorm lang; selbst unter Rückflusskochen
werden für
die Umsetzung von 27 g Aluminium 12 Stunden benötigt. Zwar lässt sich
dieser Zeitraum gemäß
Als
Verfahren für
die Herstellung von gesponnenen Fasern wird in der
Der vorliegenden Erfindung liegt die Aufgabe zugrunde, eine über längere Zeit lagerbare, chloridfreie, vorzugsweise nitratfreie Spinnmasse zur Herstellung von Stapel- und anderen Fasern im System Al2O3 oder Al2O3-SiO2 mit einem Aluminiumoxidgehalt höher als 60 %, bezogen auf den Gesamtoxidgehalt, bereitzustellen, die sich auf eine Viskosität von ca. 1,5 bis 10, vorzugsweise 2,0 – 8,0 Pas einstellen lässt und mit dieser Viskosität in einem Trockenspinnverfahren/Zentrifugalspinnverfahren verspinnbar ist.The present invention is based on the object, a storable over a long time, chloride-free, preferably nitrate-free spinning mass for the production of staple and other fibers in the system Al 2 O 3 or Al 2 O 3 -SiO 2 with an alumina content higher than 60% to provide the total oxide content, which can be adjusted to a viscosity of about 1.5 to 10, preferably 2.0 to 8.0 Pas and is spinnable with this viscosity in a dry spinning / centrifugal spinning process.
Diese Aufgabe wird gelöst durch die Bereitstellung einer spinnfähigen Masse, die erhältlich ist durch Umsetzen eines Aluminiumtriacylats, ausgewählt insbesondere unter Formiaten, Acetaten, Propionaten und Butyraten sowie Mischungen davon, mit einer Säure, die Acylatgruppen aus dem Triacylat verdrängen kann. Wenn das System außerdem Silicium enthalten soll, wird die bei dieser Umsetzung gewonnene Lösung oder Suspension mit einem SiO2-haltigen Gel oder Sol vermischt.This object is achieved by providing a spinnable composition which is obtainable by reacting an aluminum triacylate, selected in particular from formates, acetates, propionates and butyrates and mixtures thereof, with an acid which can displace acylate groups from the triacylate. If the system is also to contain silicon, the solution or suspension obtained in this reaction is mixed with an SiO 2 -containing gel or sol.
Erfindungsgemäß wird es möglichst vermieden, einen basischen oder nitrathaltigen Aluminium-Precursor zu verwenden. Darüber hinaus muß natürlich die Chloridfreiheit der SiO2-Quelle und aller sonstigen Zusatz- und Hilfsstoffe gewährleistet sein.According to the invention, it is avoided as far as possible to use a basic or nitrate-containing aluminum precursor. In addition, of course, the absence of chloride of SiO 2 source and all other additives and auxiliaries must be guaranteed.
Der Aluminium-Precursor kann entweder in Form eines Heteroacylates (-carboxylates) oder eines Homoacylates (-carboxylates) eingesetzt werden. Beispiele sind Aluminiumformiatacetat, Aluminiumformiatpropionat oder Aluminiumtriformiat.Of the Aluminum precursor can be either in the form of a heteroacylate (carboxylate) or a homoacylate (carboxylate). Examples are aluminum formate acetate, aluminum formate propionate or aluminum triformate.
Die Acylatgruppen aus dem Aluminiumtriacylat verdrängende Säure ist vorzugsweise ausgewählt unter Carbonsäuren mit einem pKs-Wert von unter 3,75. Ganz besonders bevorzugt handelt es sich um eine chelatbildenden Carbonsäure. Besonders bevorzugt ist der Einsatz von Carbonsäuren mit einem pKs-Wert von unter 2,5, noch stärker bevorzugt von unter 1.5. Carbonsäuren mit solchen Säurestärken weisen neben der Carboxygruppe meist eine oder mehrere elektronenziehende Gruppen auf wie weitere Carboxylatgruppen, Hydroxygruppen oder Ketogruppen. Besonders bevorzugt sind Di- oder Polycarbonsäuren.The Acylate groups from the aluminum triacylate displacing acid is preferably selected from carboxylic acids with a pKs value of less than 3.75. Very particularly preferred is it is a chelating carboxylic acid. Particularly preferred the use of carboxylic acids with a pKs less than 2.5, even more preferably less than 1.5. carboxylic acids show with such acid strengths in addition to the carboxy group usually one or more electron-withdrawing Groups such as other carboxylate groups, hydroxy groups or keto groups. Particularly preferred are di- or polycarboxylic acids.
Wird der verspinnbaren Masse ein Spinnhilfsmittel zugesetzt wie aus dem Stand der Technik bekannt, kann in manchen Fällen deren Verspinnbarkeit noch gesteigert werden. Als Spinnhilfsmittel können beispielsweise Milchsäure, Polyethylenoxid oder Polyvinylalkohol (PVA) dienen. Mengen von z.B. 1 bis 5, insbesondere von etwa 2,5 Masse-% an Spinnhilfsmittel wie PVA, bezogen auf die Spinnmasse, sind gut geeignet; manchmal können aber auch deutlich geringere Mengen genügen, z.B. dann, wenn Milchsäure verwendet wird.Becomes the spinnable mass added a spin aid as from the State of the art, in some cases, their spinnability be increased. As a spinning aid, for example, lactic acid, polyethylene oxide or polyvinyl alcohol (PVA). Quantities of e.g. 1 to 5, in particular of about 2.5% by weight of spinning aids such as PVA, based on the Dope, are well suited; sometimes, however, can be much lower Quantities are enough, e.g. then, if lactic acid is used.
Die
erfindungsgemäße Spinnmasse
ist mit dem Verfahren und der Anlage zu Grünfasern verspinnbar, wie sie
prinzipiell in der
Die
Erfinder mussten feststellen, dass es nicht gelingt, eine lagerstabile,
verspinnbare Masse mit den gewünschten
Eigenschaften zu erhalten, wenn man der Lehre der
Interessanterweise konnten aus der Mischung einer solchen Aluminium-Mischacylat-Lösung mit einem Kieselsol nach dem Einengen, also auch ohne Zugabe von Spinnhilfsmittel, mit Hilfe eines Glasstabes zwar Fäden gezogen werden, und das Fadenbildungsvermögen verbesserte sich durch Zugabe von Spinnhilfsmittel erwartungsgemäß. Ohne den Zusatz einer acylatverdrängenden Säure, z.B. einer chelatbildenden Säure oder einer Säure mit niedrigem pKs-Wert, konnten diese Ansätze jedoch nicht auf einer industriellen Zentrifugalspinnmaschine zu Fasern versponnen werden. Die auf diesem Wege erhaltenen Formiat-Acetat-Spinnmassen in Gegenwart von gealtertem Kieselsol verloren zudem durch Niederschlagsbildung ihr Fadenbildungsvermögen (Glasstab) bereits nach wenigen Tagen. Die Lösungen konnten auch durch Spinnhilfsmittel nicht weiter stabilisiert werden.Interestingly, could be made from the mixture of such an aluminum mixed acylate solution with a silica sol after concentration, that is also without addition of spinning aid, threads are pulled with the help of a glass rod, and that Thread-forming ability improved as expected by the addition of spin aid. Without the addition of an acylatverdrängenden Acid, e.g. a chelating acid or an acid with low pKs value, however, these approaches failed industrial centrifugal spinning machine are spun into fibers. The obtained in this way formate acetate spinning masses in the presence of aged silica also lost its precipitates Thread-forming ability (Glass rod) already after a few days. The solutions could not by spinning aids either be further stabilized.
Erfindungsgemäß stellte sich jedoch heraus, dass die Spinnmassen dann über einen längeren Zeitraum hinweg gelagert werden können, ohne ihr Fadenbildungsvermögen zu verlieren, und darüber hinaus so gute Verspinneigenschaften aufweisen, dass sie auch nach längerer Lagerungszeit auf den hier in Rede stehenden Trockenspinnanlagen versponnen werden können, wenn das eingesetzte Aluminiumtriacylat (Homo- oder Mischacylat) mit mindestens einer Carbonsäure umgesetzt wird, die zumindest einen Teil der Acylatgruppen aus dem Aluminiumtriacylat verdrängen kann. Hierfür sind chelatbildende Säuren oder Säuren mit relativ geringem pKs-Wert geeignet, z.B. Citronensäure oder Oxalsäure. Der Einsatz beider Säuren wurde detailliert untersucht; man erhielt stabile Sole, aus denen nach SiO2-Solzugabe mit anschließendem starkem Einengen auch ohne Spinnhilfsmittel mit Hilfe des Glasstab-Ziehversuchs Fäden gezogen werden konnten. Sie sind im Unterschied zu ihren Vorgängern über mehrere Wochen verwendbar, wobei das Fadenbildungsvermögen bei Ansätzen unter Verwendung von Oxalsäure gegenüber Ansätzen unter Verwendung von Citronensäure deutlich besser ist. Allerdings setzt die Fadenbildungseigenschaft oxalsäurehaltiger Spinnmassen erst bei höheren Viskositäten ein als diejenige von citronensäurehaltigen Spinnmassen.According to the invention, however, it turned out that the spinning masses can then be stored for a long period of time without losing their thread-forming ability, and moreover have such good spinning properties that they can be spun even after prolonged storage on the dry spinning plants in question here, if the aluminum triacylate used (Homo - or Mischacylat) is reacted with at least one carboxylic acid which can displace at least a portion of the Acylatgruppen from the aluminum triacylate. For this purpose, chelating acids or acids with a relatively low pKs value are suitable, for example citric acid or oxalic acid. The use of both acids has been studied in detail; Stable sols were obtained from which, after addition of SiO 2 with subsequent vigorous concentration, threads could also be drawn without spinning aid with the aid of the glass rod drawing test. They are useful in contrast to their predecessors over several weeks, with the thread-forming capacity in approaches using oxalic acid to approaches using citric acid is significantly better. However, the filament-forming property of oxalic acid-containing spinning compositions only starts at higher viscosities than that of citric acid-containing spinning compositions.
Spinnmassen mit besonders günstigen Eigenschaften erhält man, wenn man das Aluminiumtriacylat in Lösung mit der acylatverdrängenden Säure umsetzt und die Lösung anschließend bis zur Trockene eingeengt wird. Der dabei entstehende spröde Rückstand (z.B. Aluminiumformiatoxalat) hat in der Regel einen Oxidgehalt von knapp 30 Masse-%. Er kann mit Wasser oder einem wasserhaltigen, z.B. alkoholischen Lösungsmittel (unter Umständen auch in Alkoholen wie Ethanol oder Methanol, sofern die Acylatgruppen des Aluminiums weniger polar sind als Formiate) aufgenommen werden, wobei man günstigerweise eine wässrige Lösung mit ca. 5–20 Masse-% Al2O3, stärker bevorzugt mit 10–15 Masse-% Al2O3 herstellt. Dieser Lösung wird gegebenenfalls eine geeignete Menge an Kieselsol zugegeben. Die Menge wird so gewählt, dass die Spinnmasse ein Element-Verhältnis von Aluminium zu Silicium im Bereich von 1:0 bis vorzugsweise 3:2 erhält. Wenn aus der Masse Mullitfasern erzeugt werden sollen, liegt dieses Verhältnis bei etwa 3:1 oder 3:2. Nach Zugabe des Kieselsols und ggf. einem Spinnhilfsmittel lässt sich der Ansatz durch Einengen auf die erwünschte Viskosität von 1,5 bis 10 Pas, beispielsweise von ca. 3 Pas einengen. Ein solcher Ansatz lässt sich problemlos auf Trockenspinnanlagen oder Zentrifugalspinnanlagen verspinnen.Spinning compositions with particularly favorable properties are obtained by reacting the aluminum triacylate in solution with the acylate-displacing acid and then concentrating the solution to dryness. The resulting brittle residue (eg Aluminiumformiatoxalat) usually has an oxide content of nearly 30% by mass. It can be taken up with water or a water-containing, eg alcoholic, solvent (under certain circumstances also in alcohols such as ethanol or methanol, if the acylate groups of aluminum are less polar than formates), whereby an aqueous solution with approx. % Al 2 O 3 , more preferably 10-15 mass% Al 2 O 3 . Optionally, an appropriate amount of silica sol is added to this solution. The amount is chosen so that the dope obtains an elemental ratio of aluminum to silicon in the range of 1: 0 to preferably 3: 2. If mullite fibers are to be produced from the mass, this ratio is about 3: 1 or 3: 2. After addition of the silica sol and optionally a spinning aid, the mixture can be concentrated by concentration to the desired viscosity of 1.5 to 10 Pas, for example of about 3 Pas. Such an approach can be easily spun on dry spinning or centrifugal spinning equipment.
Neben der Aluminiumverbindung und gegebenenfalls Siliciumdioxid kann die erfindungsgemäße Spinnmasse bei Bedarf oder Wunsch weitere Metallverbindungen enthalten, beispielsweise Oxide von Yttrium, Zirkon, Bor und/oder Magnesium. Die Konzentration dieser Oxide sollte 10 Masse-% in der ausgeheizten Faser in Summe nicht übersteigen. Die genannten Elemente werden z.B. durch wasserlösliche Verbindungen (Acetate) in die Spinnmasse eingebracht.Next the aluminum compound and optionally silica may be the Spun mass according to the invention if required or desired, contain further metal compounds, for example Oxides of yttrium, zirconium, boron and / or magnesium. The concentration these oxides should total 10 mass% in the baked fiber do not exceed. The said elements are e.g. by water-soluble compounds (acetates) introduced into the dope.
Die Spinnmasse kann außerdem bei Bedarf geeignete Additive enthalten wie Entschäumer oder andere.The Dope can also if necessary, contain suitable additives such as defoamers or others.
Nachstehend soll die Erfindung anhand von Beispielen näher erläutert werden.below the invention will be explained in more detail by way of examples.
Beispiel 1example 1
2,226 kg Aluminiumformiat werden in 4,400 kg deionisiertes Wasser gegeben, dem dann noch 1,718 kg Eisessig hinzugefügt wurde. Nach kurzem Sieden am Rückfluss entsteht eine fast klare Lösung, die dann mit 0,976 kg eines gealterten Kieselsols mit einem Feststoffgehalt von 20,5% versetzt wird. Diese Lösung wird durch Eingengen auf 39,8 kg mit einer Oxidkonzentration von 19 Masse-% hergestellt. Die Aluminiumformiat-Oxalat-Konzentration liegt damit bei 45,6 Masse-%. Aus der Lösung lassen sich unmittelbar nach der Herstellung mit einem Glasstab Fäden ziehen. Nach wenigen Tagen wird jedoch die Bildung eines Niederschlages beobachtet, und das Fadenziehvermögen geht verloren.2,226 kg of aluminum formate are added to 4,400 kg of deionized water, which was then added 1.718 kg of glacial acetic acid. After a short simmer at reflux creates an almost clear solution that then 0.976 kg of an aged silica sol having a solids content offset by 20.5%. This solution is determined by mixing to 39.8 kg with an oxide concentration of 19 mass% produced. The aluminum formate oxalate concentration is thus 45.6% by mass. From the solution can be directly After making, use a glass rod to pull threads. After a few days However, the formation of a precipitate is observed, and the thread pull goes lost.
Beispiel 2Example 2
121,4 g Aluminiumformiat (23,0 Masse-% Aluminuimoxid) werden mit 69,76 g Oxalsäure und 240 g deion. Wasser 10 Minuten am Rückfluß gekocht. Die entstehende klare Lösung wird bei verminderten Druck eingeengt, bis sich ein viskoser Rückstand bildet. Dieser wird in einem Umlufttrockenschrank bei 200 °C getrocknet, bis ein spröder, leicht gelblicher Rückstand entsteht. Dieser wird mit 185 g deion. Wasser durch Kochen am Rückfluß in Lösung gebracht. Nach Abkühlung auf Raumtemperatur wird 53,0 g Kieselsol (20,5 Masse-% Siliciumoxid) und 33,7 g PVA-Lösung zugegeben. Bei vermindertem Druck und einer maximalen Temperatur von 60 °C wird der Ansatz eingeengt auf ca. 19 Masse-Oxidgehalt. Das Molverhältnis von Al:Si liegt in dieser Spinnmasse bei 3:1, das Massenverhältnis von Al2O3:SiO2 bei 72:28.121.4 g of aluminum formate (23.0% by mass of aluminum oxide) are mixed with 69.76 g of oxalic acid and 240 g of deion. Water boiled for 10 minutes at reflux. The resulting clear solution is concentrated at reduced pressure until a viscous residue forms. This is dried in a convection oven at 200 ° C until a brittle, slightly yellowish residue. This one comes with 185 g deion. Water is brought into solution by boiling at reflux. After cooling to room temperature, 53.0 g of silica sol (20.5% by mass of silica) and 33.7 g of PVA solution are added. At reduced pressure and a maximum temperature of 60 ° C, the mixture is concentrated to about 19 mass oxide content. The molar ratio of Al: Si in this spinning mass is 3: 1, the mass ratio of Al 2 O 3 : SiO 2 at 72:28.
Beispiel 3Example 3
Beispiel
2 wird wiederholt, wobei jedoch 23,67 kg Aluminiumformiat (Oxidgehalt
23,0) mit 13,57 kg Oxalsäure
umgesetzt wird. Nach Trocknen ergibt sich für das entstandene Aluminiumformiatoxalat
ein Oxidgehalt von 29,5 Masse-%. Durch 27,68 kg Wasserzugabe wird
eine wässrige
Lösung
mit 11,8 Masse-% Al2O3 hergestellt.
Hierzu werden 10,378 kg eines ca. 20%igen SiO2-Sols gegeben. Nach
Zugabe von 6,4 kg PVA-Lösung
und wenigen Gramm Entschäumer
liegen folgende Konzentrationen vor:
Gesamtoxidgehalt: 12,0
Masse-% (8,65 Masse-% Al2O3 und
3,30 Masse-% SiO2). Dies entspricht einem Masseverhältnis Al2O3 zu SiO2 von 72 zu 28 und einem Elementverhältnis von
3:1. Die Aluminiumformiatoxalat-Konzentration beträgt in dieser
Lösung
28,8 Masse-%.Example 2 is repeated except that 23.67 kg of aluminum formate (oxide content 23.0) is reacted with 13.57 kg of oxalic acid. After drying, the resulting aluminum formate oxalate gives an oxide content of 29.5% by mass. By 27.68 kg of water, an aqueous solution with 11.8% by weight of Al 2 O 3 is prepared. For this purpose, 10.378 kg of an approximately 20% SiO 2 sol are added. After adding 6.4 kg of PVA solution and a few grams of defoamer, the following concentrations are present:
Total Oxide Content: 12.0 mass% (8.65 mass% Al 2 O 3 and 3.30 mass% SiO 2 ). This corresponds to a mass ratio Al 2 O 3 to SiO 2 of 72 to 28 and an element ratio of 3: 1. The Aluminiumformiatoxalat concentration in this solution is 28.8% by mass.
Beispiel 4Example 4
Aus den Ansätzen der Beipiele 2 und 3 werden auf herkömmliche Weise Grünfasern gezogen, die bei Raumtemperatur getrocknet werden. Die getrockneten Gelfasern werden in einen Tiegel gebracht und innerhalb von 13 Stunden auf 1.300°C erhitzt. Nach einer Stunde bei 1.300°C lässt man die Fasern im Ofen auf Raumtemperatur abkühlen. Man erhält farblose, mechanisch stabile Fasern.Out the approaches Examples 2 and 3 are green fibers in a conventional manner pulled, which are dried at room temperature. The dried ones Gel fibers are placed in a crucible and within 13 hours at 1,300 ° C heated. After one hour at 1300 ° C, the fibers are left in the oven cool to room temperature. You get colorless, mechanically stable fibers.
Claims (16)
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DE200410026260 DE102004026260A1 (en) | 2004-05-28 | 2004-05-28 | New spinnable mass, obtained by reacting aluminum triacylate with carbonic acid and mixing with silicon dioxide containing solution, useful for preparing green fibers and/or ceramic fibers based on aluminum oxide |
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE102007018147A1 (en) * | 2007-04-16 | 2008-10-23 | Clariant International Ltd. | Spinning mass for the production of oxide ceramic fibers |
DE102008052169A1 (en) | 2007-10-27 | 2009-04-30 | Bayerische Motoren Werke Aktiengesellschaft | Producing ceramic oxide fiber comprises spinning a spinning mass comprising ceramic oxide forming component and organic polymers; sintering the obtained green fiber to ceramic oxide fiber |
Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE2054573B2 (en) * | 1970-11-06 | 1978-10-26 | Bayer Ag, 5090 Leverkusen | Inorganic fibers and processes for their manufacture |
WO1992001644A1 (en) * | 1990-07-23 | 1992-02-06 | Akzo N.V. | Aluminium oxide fibres and process for producing them |
-
2004
- 2004-05-28 DE DE200410026260 patent/DE102004026260A1/en not_active Ceased
Patent Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE2054573B2 (en) * | 1970-11-06 | 1978-10-26 | Bayer Ag, 5090 Leverkusen | Inorganic fibers and processes for their manufacture |
WO1992001644A1 (en) * | 1990-07-23 | 1992-02-06 | Akzo N.V. | Aluminium oxide fibres and process for producing them |
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE102007018147A1 (en) * | 2007-04-16 | 2008-10-23 | Clariant International Ltd. | Spinning mass for the production of oxide ceramic fibers |
DE102008052169A1 (en) | 2007-10-27 | 2009-04-30 | Bayerische Motoren Werke Aktiengesellschaft | Producing ceramic oxide fiber comprises spinning a spinning mass comprising ceramic oxide forming component and organic polymers; sintering the obtained green fiber to ceramic oxide fiber |
DE102008052169B4 (en) * | 2007-10-27 | 2013-07-18 | Bayerische Motoren Werke Aktiengesellschaft | Process for the preparation of oxide ceramic fibers and use of fibers produced therefrom |
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