JP5231553B2 - 透明で安定な二酸化チタンゾル - Google Patents
透明で安定な二酸化チタンゾル Download PDFInfo
- Publication number
- JP5231553B2 JP5231553B2 JP2010523170A JP2010523170A JP5231553B2 JP 5231553 B2 JP5231553 B2 JP 5231553B2 JP 2010523170 A JP2010523170 A JP 2010523170A JP 2010523170 A JP2010523170 A JP 2010523170A JP 5231553 B2 JP5231553 B2 JP 5231553B2
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- Prior art keywords
- sol
- titanium dioxide
- titanium
- transparent
- stable
- 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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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims description 137
- 239000004408 titanium dioxide Substances 0.000 title claims description 56
- 238000000034 method Methods 0.000 claims description 29
- 239000010936 titanium Substances 0.000 claims description 25
- 229910052719 titanium Inorganic materials 0.000 claims description 25
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 23
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 19
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 claims description 18
- VXUYXOFXAQZZMF-UHFFFAOYSA-N titanium(IV) isopropoxide Chemical compound CC(C)O[Ti](OC(C)C)(OC(C)C)OC(C)C VXUYXOFXAQZZMF-UHFFFAOYSA-N 0.000 claims description 18
- 150000001875 compounds Chemical class 0.000 claims description 17
- 230000001699 photocatalysis Effects 0.000 claims description 17
- 239000006185 dispersion Substances 0.000 claims description 16
- 239000002245 particle Substances 0.000 claims description 16
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 15
- 239000008367 deionised water Substances 0.000 claims description 12
- 229910021641 deionized water Inorganic materials 0.000 claims description 12
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 claims description 9
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 claims description 9
- 239000004310 lactic acid Substances 0.000 claims description 9
- 235000014655 lactic acid Nutrition 0.000 claims description 9
- 239000011975 tartaric acid Substances 0.000 claims description 9
- 235000002906 tartaric acid Nutrition 0.000 claims description 9
- 230000007935 neutral effect Effects 0.000 claims description 8
- -1 titanium alkoxide Chemical class 0.000 claims description 8
- 229910000349 titanium oxysulfate Inorganic materials 0.000 claims description 7
- 239000002253 acid Substances 0.000 claims description 6
- 230000002378 acidificating effect Effects 0.000 claims description 6
- XFVGXQSSXWIWIO-UHFFFAOYSA-N chloro hypochlorite;titanium Chemical compound [Ti].ClOCl XFVGXQSSXWIWIO-UHFFFAOYSA-N 0.000 claims description 4
- 235000015165 citric acid Nutrition 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- BJEPYKJPYRNKOW-REOHCLBHSA-N (S)-malic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O BJEPYKJPYRNKOW-REOHCLBHSA-N 0.000 claims description 3
- ADVORQMAWLEPOI-XHTSQIMGSA-N (e)-4-hydroxypent-3-en-2-one;oxotitanium Chemical compound [Ti]=O.C\C(O)=C/C(C)=O.C\C(O)=C/C(C)=O ADVORQMAWLEPOI-XHTSQIMGSA-N 0.000 claims description 3
- BJEPYKJPYRNKOW-UHFFFAOYSA-N alpha-hydroxysuccinic acid Natural products OC(=O)C(O)CC(O)=O BJEPYKJPYRNKOW-UHFFFAOYSA-N 0.000 claims description 3
- 239000001630 malic acid Substances 0.000 claims description 3
- 235000011090 malic acid Nutrition 0.000 claims description 3
- 230000001376 precipitating effect Effects 0.000 claims description 3
- 150000007513 acids Chemical class 0.000 claims description 2
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 2
- 150000002334 glycols Chemical class 0.000 claims 1
- 230000003472 neutralizing effect Effects 0.000 claims 1
- 238000005406 washing Methods 0.000 claims 1
- 239000000243 solution Substances 0.000 description 15
- 238000000576 coating method Methods 0.000 description 11
- 239000000758 substrate Substances 0.000 description 11
- 229910002089 NOx Inorganic materials 0.000 description 9
- 229910010413 TiO 2 Inorganic materials 0.000 description 9
- 238000001556 precipitation Methods 0.000 description 9
- 238000003756 stirring Methods 0.000 description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 8
- AEMRFAOFKBGASW-UHFFFAOYSA-N Glycolic acid Chemical compound OCC(O)=O AEMRFAOFKBGASW-UHFFFAOYSA-N 0.000 description 8
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 8
- 239000002105 nanoparticle Substances 0.000 description 8
- 239000002244 precipitate Substances 0.000 description 8
- 239000000203 mixture Substances 0.000 description 7
- MWUXSHHQAYIFBG-UHFFFAOYSA-N Nitric oxide Chemical compound O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 6
- 239000011248 coating agent Substances 0.000 description 6
- 239000000356 contaminant Substances 0.000 description 6
- 230000007062 hydrolysis Effects 0.000 description 6
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- 238000002173 high-resolution transmission electron microscopy Methods 0.000 description 5
- 238000005259 measurement Methods 0.000 description 5
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- 239000000047 product Substances 0.000 description 5
- 239000002904 solvent Substances 0.000 description 5
- YBRBMKDOPFTVDT-UHFFFAOYSA-N tert-butylamine Chemical compound CC(C)(C)N YBRBMKDOPFTVDT-UHFFFAOYSA-N 0.000 description 5
- 238000004140 cleaning Methods 0.000 description 4
- 239000010408 film Substances 0.000 description 4
- 238000004627 transmission electron microscopy Methods 0.000 description 4
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 3
- 235000011114 ammonium hydroxide Nutrition 0.000 description 3
- 230000008901 benefit Effects 0.000 description 3
- 239000000919 ceramic Substances 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000000386 microscopy Methods 0.000 description 3
- DCKVFVYPWDKYDN-UHFFFAOYSA-L oxygen(2-);titanium(4+);sulfate Chemical compound [O-2].[Ti+4].[O-]S([O-])(=O)=O DCKVFVYPWDKYDN-UHFFFAOYSA-L 0.000 description 3
- 238000010979 pH adjustment Methods 0.000 description 3
- 239000002243 precursor Substances 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- 239000003381 stabilizer Substances 0.000 description 3
- KBPLFHHGFOOTCA-UHFFFAOYSA-N 1-Octanol Chemical compound CCCCCCCCO KBPLFHHGFOOTCA-UHFFFAOYSA-N 0.000 description 2
- BBMCTIGTTCKYKF-UHFFFAOYSA-N 1-heptanol Chemical compound CCCCCCCO BBMCTIGTTCKYKF-UHFFFAOYSA-N 0.000 description 2
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 2
- AMQJEAYHLZJPGS-UHFFFAOYSA-N N-Pentanol Chemical compound CCCCCO AMQJEAYHLZJPGS-UHFFFAOYSA-N 0.000 description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 2
- 238000003917 TEM image Methods 0.000 description 2
- 239000004809 Teflon Substances 0.000 description 2
- 229920006362 Teflon® Polymers 0.000 description 2
- 229910052768 actinide Inorganic materials 0.000 description 2
- 150000001255 actinides Chemical class 0.000 description 2
- 229940061720 alpha hydroxy acid Drugs 0.000 description 2
- 150000001280 alpha hydroxy acids Chemical class 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 239000003637 basic solution Substances 0.000 description 2
- 238000005202 decontamination Methods 0.000 description 2
- 230000003588 decontaminative effect Effects 0.000 description 2
- 230000001747 exhibiting effect Effects 0.000 description 2
- 239000012065 filter cake Substances 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- ZSIAUFGUXNUGDI-UHFFFAOYSA-N hexan-1-ol Chemical compound CCCCCCO ZSIAUFGUXNUGDI-UHFFFAOYSA-N 0.000 description 2
- 150000002603 lanthanum Chemical class 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 229910021645 metal ion Inorganic materials 0.000 description 2
- 238000006386 neutralization reaction Methods 0.000 description 2
- 229910017604 nitric acid Inorganic materials 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 description 2
- 230000000737 periodic effect Effects 0.000 description 2
- 230000005855 radiation Effects 0.000 description 2
- 239000000725 suspension Substances 0.000 description 2
- WGTYBPLFGIVFAS-UHFFFAOYSA-M tetramethylammonium hydroxide Chemical compound [OH-].C[N+](C)(C)C WGTYBPLFGIVFAS-UHFFFAOYSA-M 0.000 description 2
- 150000003609 titanium compounds Chemical class 0.000 description 2
- 239000012855 volatile organic compound Substances 0.000 description 2
- RYSXWUYLAWPLES-MTOQALJVSA-N (Z)-4-hydroxypent-3-en-2-one titanium Chemical compound [Ti].C\C(O)=C\C(C)=O.C\C(O)=C\C(C)=O.C\C(O)=C\C(C)=O.C\C(O)=C\C(C)=O RYSXWUYLAWPLES-MTOQALJVSA-N 0.000 description 1
- GRWPYGBKJYICOO-UHFFFAOYSA-N 2-methylpropan-2-olate;titanium(4+) Chemical compound [Ti+4].CC(C)(C)[O-].CC(C)(C)[O-].CC(C)(C)[O-].CC(C)(C)[O-] GRWPYGBKJYICOO-UHFFFAOYSA-N 0.000 description 1
- MGWGWNFMUOTEHG-UHFFFAOYSA-N 4-(3,5-dimethylphenyl)-1,3-thiazol-2-amine Chemical compound CC1=CC(C)=CC(C=2N=C(N)SC=2)=C1 MGWGWNFMUOTEHG-UHFFFAOYSA-N 0.000 description 1
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonium chloride Substances [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 1
- 239000007848 Bronsted acid Substances 0.000 description 1
- 241000195493 Cryptophyta Species 0.000 description 1
- 241000221785 Erysiphales Species 0.000 description 1
- 229910002651 NO3 Inorganic materials 0.000 description 1
- OUUQCZGPVNCOIJ-UHFFFAOYSA-M Superoxide Chemical compound [O-][O] OUUQCZGPVNCOIJ-UHFFFAOYSA-M 0.000 description 1
- 230000006750 UV protection Effects 0.000 description 1
- 150000001339 alkali metal compounds Chemical class 0.000 description 1
- 150000004703 alkoxides Chemical class 0.000 description 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Natural products N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 1
- 239000000908 ammonium hydroxide Substances 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000003899 bactericide agent Substances 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 description 1
- 125000002843 carboxylic acid group Chemical group 0.000 description 1
- 150000001735 carboxylic acids Chemical class 0.000 description 1
- 239000004568 cement Substances 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 239000002738 chelating agent Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000002242 deionisation method Methods 0.000 description 1
- HPNMFZURTQLUMO-UHFFFAOYSA-N diethylamine Chemical compound CCNCC HPNMFZURTQLUMO-UHFFFAOYSA-N 0.000 description 1
- 238000010494 dissociation reaction Methods 0.000 description 1
- 230000005593 dissociations Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000005357 flat glass Substances 0.000 description 1
- 239000000499 gel Substances 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- TUJKJAMUKRIRHC-UHFFFAOYSA-N hydroxyl Chemical compound [OH] TUJKJAMUKRIRHC-UHFFFAOYSA-N 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 150000007529 inorganic bases Chemical class 0.000 description 1
- 239000010985 leather Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000004579 marble Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- JCXJVPUVTGWSNB-UHFFFAOYSA-N nitrogen dioxide Inorganic materials O=[N]=O JCXJVPUVTGWSNB-UHFFFAOYSA-N 0.000 description 1
- 150000007524 organic acids Chemical class 0.000 description 1
- 150000007530 organic bases Chemical class 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000003002 pH adjusting agent Substances 0.000 description 1
- 239000000123 paper Substances 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000011941 photocatalyst Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- HKJYVRJHDIPMQB-UHFFFAOYSA-N propan-1-olate;titanium(4+) Chemical compound CCCO[Ti](OCCC)(OCCC)OCCC HKJYVRJHDIPMQB-UHFFFAOYSA-N 0.000 description 1
- RLJWTAURUFQFJP-UHFFFAOYSA-N propan-2-ol;titanium Chemical compound [Ti].CC(C)O.CC(C)O.CC(C)O.CC(C)O RLJWTAURUFQFJP-UHFFFAOYSA-N 0.000 description 1
- 239000011541 reaction mixture Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000003352 sequestering agent Substances 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 241000894007 species Species 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 229910052861 titanite Inorganic materials 0.000 description 1
- JMXKSZRRTHPKDL-UHFFFAOYSA-N titanium ethoxide Chemical compound [Ti+4].CC[O-].CC[O-].CC[O-].CC[O-] JMXKSZRRTHPKDL-UHFFFAOYSA-N 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
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- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/60—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only artificial stone
- C04B41/61—Coating or impregnation
- C04B41/65—Coating or impregnation with inorganic materials
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- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/06—Silicon, titanium, zirconium or hafnium; Oxides or hydroxides thereof
- B01J21/063—Titanium; Oxides or hydroxides thereof
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- B01J35/20—Catalysts, in general, characterised by their form or physical properties characterised by their non-solid state
- B01J35/23—Catalysts, in general, characterised by their form or physical properties characterised by their non-solid state in a colloidal state
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- B01J35/39—Photocatalytic properties
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- B01J37/0215—Coating
- B01J37/0219—Coating the coating containing organic compounds
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/04—Oxides; Hydroxides
- C01G23/047—Titanium dioxide
- C01G23/053—Producing by wet processes, e.g. hydrolysing titanium salts
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C1/00—Ingredients generally applicable to manufacture of glasses, glazes, or vitreous enamels
- C03C1/006—Ingredients generally applicable to manufacture of glasses, glazes, or vitreous enamels to produce glass through wet route
- C03C1/008—Ingredients generally applicable to manufacture of glasses, glazes, or vitreous enamels to produce glass through wet route for the production of films or coatings
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
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- C03C17/02—Surface treatment of glass, not in the form of fibres or filaments, by coating with glass
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- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
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- C04B41/009—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone characterised by the material treated
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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
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/50—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials
- C04B41/5025—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials with ceramic materials
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- C01P2004/00—Particle morphology
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
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- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
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- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2218/00—Methods for coating glass
- C03C2218/10—Deposition methods
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Description
(i)チタン含有化合物、例えば、チタンアルコキシド、オキシ塩化チタン、硫酸チタニル、またはチタニルアセチルアセトナートを含む溶液を準備し;
(ii)チタン含有化合物の該溶液から含水二酸化チタンを沈殿させ;
(iii)沈殿した含水二酸化チタンの水性分散液を形成し;ついで
(iv)1またはそれを超えるアルファ−ヒドロキシカルボン酸、例えば、乳酸、酒石酸、リンゴ酸、クエン酸およびそれらの組み合わせの存在下、約70℃ないし約150℃の温度にて約3時間ないし約3日間、該水性分散液を混合することを含む、安定で透明な光触媒二酸化チタンゾルを調製するための方法を提供する。1またはそれを超えるアルファ−ヒドロキシカルボン酸は、高温処理工程の間に存在することが要求されるが、それらを工程(i)−(iv)のいずれの工程の間にも導入できることは理解されるであろう。本発明の1の変形において、高温処理は有利には先の中和工程なしに有利に行う。もう1の変形において、該1またはそれを超えるアルファ−ヒドロキシカルボン酸にはグリコール酸は含まれないであろう。
本発明にかかる透明な二酸化チタンゾルは、次のようにして調製した。50gのイソプロパノールで希釈した50gのチタンイソプロポキシド(Alfa Aesar、95%)を、強く攪拌しながら250gの脱イオン水に徐々に添加した。二酸化チタンが沈殿した後、さらに約10分間攪拌を維持した。ついで、沈澱物を濾過し、500gの脱イオン水で洗浄した。洗浄した湿式濾過ケーキは、脱イオン水に再分散して総重量250gの分散液に再分散した。6gの乳酸(Alfa Aesar、水中の85%)を分散液に添加し、よく混合した。その分散液を、テフロン製のキャップおよび蓋とともに並べた爆弾型の熱水反応器(125ml容量、Parr Instruments)に満たした。ついで、その爆弾型の反応器を、25RPMの回転速度および80℃の温度設定のローラー式乾燥機に入れた。処理は24時間維持した。ゾルを室温まで冷却した後、そのpHは2.3であった。tert−ブチルアミン(Alfa Aesar、98%)をゾルに添加してpHを7.0に調整した。最終的なゾル生成物は安定かつ完全に透明であり、TEM検鏡はそれが<5nmの結晶性TiO2ナノ粒子を含むことを明らかにした。高分解能TEM像のd−spaceの測定は、大部分のクリスタライトが、二次相としてルチル(<50%)を含むアナターゼ(>50%)であることを示した。
乳酸の代わりに7.6gの硝酸(69重量%溶液)を解膠剤として使用した以外は実施例1に記載したのと同じ方法によって試料を調整した。解膠後、ゾルは安定のようであったが、乳白色の不透明な外観を有していた。
解膠剤として乳酸の代わりに4.5gの酒石酸(Alfa Aesar、99%)を用いる以外は、実施例1と同じ方法を用いて本発明にかかる透明な二酸化チタンゾルを調製した。得られたゾルは安定かつ透明であった。TEM検鏡は、それが<5nmのTiO2ナノ粒子を含むことを明らかにした。高分解能TEM d−space測定は、大部分のクリスタライトが〜0.6nmの通常ない大きなd−spaceを示す未知の二次相(<50%)を含むアナターゼ(>50%)であることを明らかにした。
解膠剤として乳酸の代わりに10.5gのクエン酸を用い、解膠処理を3日間維持した以外は、実施例1と同じ方法を用いて本発明にかかる透明な二酸化チタンゾルを調製した。得られたゾルは安定かつ透明であった。TEM検鏡は、それが<5nmのTiO2ナノ粒子を含むことを明らかにした。高分解能TEM d−space測定は、大部分のクリスタライトが〜0.6nmの通常ない大きなd−spaceを示す未知の二次相(<50%)を含むアナターゼ(>50%)であることを明らかにした。
4.0gの乳酸を用い、解膠を熱水条件下、120℃で2日間行った以外は、実施例1と同じ方法を用いて本発明にかかる透明な二酸化チタンゾルを調製した。酸性ゾルを、tert−ブチルアミンでpH8.0に中和した。ゾル生成物は安定かつ透明であった。TEM像はよく結晶化した5nmのTiO2ナノ粒子を示した。高分解能TEM像上のd−space測定は、大部分のクリスタライトが二次相(<50%)としてルチルを含むアナターゼ(>50%)であることを明らかにした。
6.0gの酒石酸を用い、解膠を熱水条件下、120℃で2日間行った以外は、実施例1と同じ方法を用いて本発明にかかる透明な二酸化チタンゾルを調製した。酸性ゾルを、tert−ブチルアミンでpH8.0に中和した。ゾル生成物は安定かつ透明であった。TEM像はよく結晶化した5nmのTiO2ナノ粒子を示した。高分解能TEM像上のd−space測定は、大部分のクリスタライトがから0.6nmの通常ない大きなd−spaceを示す未知の二次相(<50%)を含むアナターゼ(>50%)であることを明らかにした。
本発明にかかる透明な二酸化チタンゾルを次のようにして調製した。50gのチタンイソプロポキシドを、酒石酸のイソプロパノール溶液(100gのイソプロパノール中の12.5gの酒石酸)と混合した。この混合物に、強く攪拌しながら125gの脱イオン水に徐々に添加した。加水分解後、攪拌を15分間維持し、その後に遠心によって沈殿を分離し、上層の液体層を静かに除いた。湿式固体層を水に再分散して総重量を250gとした。それを爆弾型反応器に満たし、ローラー式乾燥機中、80℃にて3日間処理した。調製した約2.0のpHを有するゾル試料をtert−ブチルアミンでpH8.0に調整した。それは安定かつ透明であった。
この実施例では、実施例5のゾルの大スケール調製を提供する。試料は、125mlの爆弾型反応器の代わりにヒーター、テフロン製ライナーおよび磁気作動スターラーを備えた2リットル熱水反応器を試料調製に用いる以外は実施例5で使用したものと同じであった。この反応器を用いて、約1.5kgの試料を各バッチで得た。外観、特性および光触媒性能は実施例5と実質的に同じであった。
この実施例では、TiO2前駆体としてオキシ硫酸チタン(TiOSO4)を用い、TiO2の沈殿をアンモニア水を用いたpH調整によって影響した。水中の950gのオキシ硫酸チタン(TiO2分析に基づいて7.9%、Millennium Inorganic Chemicals)を、950gの脱イオン水を含む4Lビーカーに25ml/分で添加した。同時に、沈殿工程全体を通して反応混合物のpHが約8.0に維持される速度で、アンモニア溶液(29%)をビーカーに添加した。沈澱物をさらに30分間攪拌した後に、それを濾過し、5Lの脱イオン水で洗浄した。ついで、洗浄した湿式沈澱物を脱イオン水を用いて再分散して分散液の総重量を約1,400gとした。45gの酒石酸を攪拌しつつ分散液に添加し、その分散液を実施例7に記載した2L熱水反応器に満たした。それを120℃にて2日間、熱水処理した。実施例5に記載した試料と同様の外観および特性を有する透明なTiO2ゾルを得た。
本発明にかかるゾルから調製したコーティングの光触媒活性を調べるために、実施例2、4、5および8のゾルをコンクリート基体上に薄層として堆積して(18cm2の領域上の約0.3mlのゾル)、各々、試料A、B、CおよびDを得た。UV線(2W/m2)下のNOx汚染物に対する活性を、約4,000時間の期間にわたって種々の間隔で測定した。NOx減少を測定する方法は、出典明示して本明細書の一部とみなす米国特許出願公開2007/0167551に実質的に記載されている。図1に示すように、各試料は全時間にわたる%NOx除去として表す実質的な(すなわち、約15%よりも大きな)光触媒活性を示した。興味深いことに、チタンイソプロポキシドの加水分解によって調製した試料A、BおよびCは時間にわたって増大する%NOx除去を示したが、オキシ硫酸チタン(TiOSO4)からpH誘導沈殿によって調製した試料Dは約1,500時間まで極めて高い(例えば、約50%ないし約75%)の初期%NOx除去を示し、徐々に約45%のNOx除去の上で平行になることを示した。
Claims (13)
- (i)チタン含有化合物を含む溶液を準備し;
(ii)チタン含有化合物の該溶液から含水二酸化チタンを沈殿させ、ついで該沈殿した含水二酸化チタンを回収し脱イオン水で洗浄し;
(iii)沈殿させた含水二酸化チタンの水性分散液を形成し;ついで
(iv)熱水反応ゾーン中、1またはそれを超えるアルファ−ヒドロキシカルボン酸の存在下、70℃ないし150℃の温度にて3時間ないし3日間、該水性分散液を混合することを含む、安定で透明な光触媒二酸化チタンゾルを調製する方法であって、但し、該1またはそれを超えるアルファ−ヒドロキシカルボン酸は実質的にグリコール酸を含まず;それによって、2ないし12のpH範囲の全体にわたる毎pHで安定かつ透明な二酸化チタンのゾルを提供し;該ゾルは10nm未満の平均粒径を有する二酸化チタンのクリスタライトを含み、該クリスタライトの大部分がアナターゼ型で存在する該方法。 - 該チタン含有化合物が、チタンアルコキシド、オキシ塩化チタン、硫酸チタニルおよびチタニルアセチルアセトナートよりなる群から選択される請求項1記載の方法。
- 該チタン含有化合物がチタンイソプロポキシドである請求項2記載の方法。
- 該1またはそれを超えるアルファ−ヒドロキシカルボン酸が、乳酸、酒石酸、リンゴ酸、クエン酸およびそれらの組み合わせよりなる群から選択されるアルファ−ヒドロキシカルボン酸を含む請求項1記載の方法。
- 該1またはそれを超えるアルファ−ヒドロキシカルボン酸が乳酸を含む請求項4記載の方法。
- 該1またはそれを超えるアルファ−ヒドロキシカルボン酸が酒石酸を含む請求項4記載の方法。
- 該1またはそれを超えるアルファ−ヒドロキシカルボン酸がクエン酸を含む請求項4記載の方法。
- さらに、得られたゾルを塩基で中和する工程を含む請求項1記載の方法。
- 該ゾルが、5nm未満の平均粒径を有する二酸化チタンクリスタライトを含む請求項1記載の方法。
- 該ゾルが、少なくとも90%がアナターゼ型で存在する二酸化チタンクリスタライトを含む請求項1記載の方法。
- 1nmないし10nmの平均クリスタライト径を有する1ないし10重量%の光触媒二酸化チタン粒子を含む安定で透明なゾルであって、該クリスタライトの大部分がアナターゼ型であり、該ゾルが酸性、中性および塩基性のpHで安定かつ透明である該ゾル。
- 該二酸化チタンクリスタライトが1nmないし5nmの平均粒径を有する請求項11記載の安定で透明なゾル。
- 該クリスタライトの少なくとも90%がアナターゼ型で存在する請求項11記載の安定で透明なゾル。
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US11/848,967 US7763565B2 (en) | 2007-08-31 | 2007-08-31 | Transparent, stable titanium dioxide sols |
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PCT/US2008/074879 WO2009029856A1 (en) | 2007-08-31 | 2008-08-29 | Transparent, stable titanium dioxide sols |
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JP2010537809A (ja) | 2010-12-09 |
UA100530C2 (ru) | 2013-01-10 |
AU2008292827A1 (en) | 2009-03-05 |
TWI413615B (zh) | 2013-11-01 |
EP2200742A4 (en) | 2016-02-24 |
CA2697542C (en) | 2012-10-23 |
WO2009029856A1 (en) | 2009-03-05 |
EP2200742A1 (en) | 2010-06-30 |
RU2010107391A (ru) | 2011-10-10 |
KR101265660B1 (ko) | 2013-05-22 |
ES2679126T3 (es) | 2018-08-22 |
EP2200742B1 (en) | 2018-07-11 |
TW200927662A (en) | 2009-07-01 |
SA08290536B1 (ar) | 2011-09-04 |
US20110183838A1 (en) | 2011-07-28 |
NZ583550A (en) | 2011-02-25 |
CN101827650B (zh) | 2013-03-20 |
US7932208B2 (en) | 2011-04-26 |
AR069730A1 (es) | 2010-02-17 |
US20100267550A1 (en) | 2010-10-21 |
CA2697542A1 (en) | 2009-03-05 |
KR20100080509A (ko) | 2010-07-08 |
BRPI0815786B1 (pt) | 2018-02-06 |
CN101827650A (zh) | 2010-09-08 |
AR101012A2 (es) | 2016-11-16 |
US20090062111A1 (en) | 2009-03-05 |
MX2010002241A (es) | 2010-03-25 |
AU2008292827B2 (en) | 2012-04-19 |
BRPI0815786A2 (pt) | 2015-02-24 |
US7763565B2 (en) | 2010-07-27 |
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