JP4101236B2 - 分散された二酸化チタンを含有する非酸性、非塩基性コロイド溶液、その製造方法及びそのコロイド溶液を含むコーティング剤 - Google Patents
分散された二酸化チタンを含有する非酸性、非塩基性コロイド溶液、その製造方法及びそのコロイド溶液を含むコーティング剤 Download PDFInfo
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- JP4101236B2 JP4101236B2 JP2004566471A JP2004566471A JP4101236B2 JP 4101236 B2 JP4101236 B2 JP 4101236B2 JP 2004566471 A JP2004566471 A JP 2004566471A JP 2004566471 A JP2004566471 A JP 2004566471A JP 4101236 B2 JP4101236 B2 JP 4101236B2
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims description 188
- 239000004408 titanium dioxide Substances 0.000 title claims description 85
- 238000004519 manufacturing process Methods 0.000 title claims description 18
- 239000011248 coating agent Substances 0.000 title description 11
- 239000000243 solution Substances 0.000 claims description 161
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 47
- AEMRFAOFKBGASW-UHFFFAOYSA-N Glycolic acid Chemical compound OCC(O)=O AEMRFAOFKBGASW-UHFFFAOYSA-N 0.000 claims description 36
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 35
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 33
- 238000000034 method Methods 0.000 claims description 32
- 239000002105 nanoparticle Substances 0.000 claims description 31
- -1 alkyl acetoacetate Chemical compound 0.000 claims description 19
- 239000003381 stabilizer Substances 0.000 claims description 19
- 150000003609 titanium compounds Chemical class 0.000 claims description 19
- 238000003756 stirring Methods 0.000 claims description 18
- 230000007935 neutral effect Effects 0.000 claims description 15
- 238000010438 heat treatment Methods 0.000 claims description 14
- 239000000203 mixture Substances 0.000 claims description 14
- 239000010936 titanium Substances 0.000 claims description 13
- 229910052719 titanium Inorganic materials 0.000 claims description 13
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 12
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 12
- 238000006243 chemical reaction Methods 0.000 claims description 12
- 239000002202 Polyethylene glycol Substances 0.000 claims description 11
- 239000003637 basic solution Substances 0.000 claims description 11
- 239000012153 distilled water Substances 0.000 claims description 11
- 229920001223 polyethylene glycol Polymers 0.000 claims description 11
- 229920002689 polyvinyl acetate Polymers 0.000 claims description 11
- 239000011118 polyvinyl acetate Substances 0.000 claims description 11
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 claims description 11
- 239000007864 aqueous solution Substances 0.000 claims description 9
- JMXKSZRRTHPKDL-UHFFFAOYSA-N titanium ethoxide Chemical compound [Ti+4].CC[O-].CC[O-].CC[O-].CC[O-] JMXKSZRRTHPKDL-UHFFFAOYSA-N 0.000 claims description 9
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 8
- QSJXEFYPDANLFS-UHFFFAOYSA-N Diacetyl Chemical compound CC(=O)C(C)=O QSJXEFYPDANLFS-UHFFFAOYSA-N 0.000 claims description 8
- 150000007514 bases Chemical class 0.000 claims description 8
- 229910052782 aluminium Inorganic materials 0.000 claims description 7
- 239000000084 colloidal system Substances 0.000 claims description 7
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 6
- UWJJYHHHVWZFEP-UHFFFAOYSA-N pentane-1,1-diol Chemical compound CCCCC(O)O UWJJYHHHVWZFEP-UHFFFAOYSA-N 0.000 claims description 6
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 6
- 150000003377 silicon compounds Chemical class 0.000 claims description 6
- YRKCREAYFQTBPV-UHFFFAOYSA-N acetylacetone Chemical compound CC(=O)CC(C)=O YRKCREAYFQTBPV-UHFFFAOYSA-N 0.000 claims description 4
- 229910021529 ammonia Inorganic materials 0.000 claims description 4
- CDQSJQSWAWPGKG-UHFFFAOYSA-N butane-1,1-diol Chemical compound CCCC(O)O CDQSJQSWAWPGKG-UHFFFAOYSA-N 0.000 claims description 4
- TZMFJUDUGYTVRY-UHFFFAOYSA-N ethyl methyl diketone Natural products CCC(=O)C(C)=O TZMFJUDUGYTVRY-UHFFFAOYSA-N 0.000 claims description 4
- WJLUBOLDZCQZEV-UHFFFAOYSA-M hexadecyl(trimethyl)azanium;hydroxide Chemical compound [OH-].CCCCCCCCCCCCCCCC[N+](C)(C)C WJLUBOLDZCQZEV-UHFFFAOYSA-M 0.000 claims description 4
- YQXQWFASZYSARF-UHFFFAOYSA-N methanol;titanium Chemical compound [Ti].OC YQXQWFASZYSARF-UHFFFAOYSA-N 0.000 claims description 4
- 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 4
- AEMRFAOFKBGASW-UHFFFAOYSA-M Glycolate Chemical compound OCC([O-])=O AEMRFAOFKBGASW-UHFFFAOYSA-M 0.000 claims description 3
- 229910052783 alkali metal Inorganic materials 0.000 claims description 3
- 229910052784 alkaline earth metal Inorganic materials 0.000 claims description 3
- 125000005210 alkyl ammonium group Chemical group 0.000 claims description 3
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 claims description 3
- 150000002506 iron compounds Chemical class 0.000 claims description 3
- 235000006408 oxalic acid Nutrition 0.000 claims description 3
- 150000003755 zirconium compounds Chemical class 0.000 claims description 3
- LCKIEQZJEYYRIY-UHFFFAOYSA-N Titanium ion Chemical compound [Ti+4] LCKIEQZJEYYRIY-UHFFFAOYSA-N 0.000 claims 2
- 150000001298 alcohols Chemical class 0.000 claims 2
- ZKWSTMNRYXEVAB-UHFFFAOYSA-N octadecanoic acid;titanium Chemical compound [Ti].CCCCCCCCCCCCCCCCCC(O)=O ZKWSTMNRYXEVAB-UHFFFAOYSA-N 0.000 claims 2
- 150000001340 alkali metals Chemical class 0.000 claims 1
- 150000001342 alkaline earth metals Chemical class 0.000 claims 1
- KKCBUQHMOMHUOY-UHFFFAOYSA-N sodium oxide Chemical compound [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 claims 1
- 229910001948 sodium oxide Inorganic materials 0.000 claims 1
- 239000010419 fine particle Substances 0.000 description 25
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 15
- 238000002835 absorbance Methods 0.000 description 9
- 239000011521 glass Substances 0.000 description 7
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 6
- 230000002776 aggregation Effects 0.000 description 6
- 238000006460 hydrolysis reaction Methods 0.000 description 6
- 239000002245 particle Substances 0.000 description 6
- 229910010413 TiO 2 Inorganic materials 0.000 description 5
- 238000004220 aggregation Methods 0.000 description 5
- 238000005259 measurement Methods 0.000 description 5
- 239000011859 microparticle Substances 0.000 description 5
- 229920000642 polymer Polymers 0.000 description 5
- 239000000047 product Substances 0.000 description 5
- 150000003839 salts Chemical class 0.000 description 5
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 4
- 239000000919 ceramic Substances 0.000 description 4
- 239000000945 filler Substances 0.000 description 4
- 230000007062 hydrolysis Effects 0.000 description 4
- 238000006386 neutralization reaction Methods 0.000 description 4
- 150000007524 organic acids Chemical class 0.000 description 4
- 150000003961 organosilicon compounds Chemical class 0.000 description 4
- 239000002904 solvent Substances 0.000 description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 230000002378 acidificating effect Effects 0.000 description 3
- 125000003158 alcohol group Chemical group 0.000 description 3
- 238000001914 filtration Methods 0.000 description 3
- 238000001027 hydrothermal synthesis Methods 0.000 description 3
- 125000000468 ketone group Chemical group 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 239000000123 paper Substances 0.000 description 3
- 239000010409 thin film Substances 0.000 description 3
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 2
- 125000000218 acetic acid group Chemical group C(C)(=O)* 0.000 description 2
- 230000004931 aggregating effect Effects 0.000 description 2
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 description 2
- WOWHHFRSBJGXCM-UHFFFAOYSA-M cetyltrimethylammonium chloride Chemical compound [Cl-].CCCCCCCCCCCCCCCC[N+](C)(C)C WOWHHFRSBJGXCM-UHFFFAOYSA-M 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 239000000835 fiber Substances 0.000 description 2
- 238000009501 film coating Methods 0.000 description 2
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 2
- 239000010985 leather Substances 0.000 description 2
- 230000003472 neutralizing effect Effects 0.000 description 2
- 229910017604 nitric acid Inorganic materials 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 235000005985 organic acids Nutrition 0.000 description 2
- 239000012266 salt solution Substances 0.000 description 2
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 2
- 238000004528 spin coating Methods 0.000 description 2
- 239000004753 textile Substances 0.000 description 2
- 239000002023 wood Substances 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- 239000002879 Lewis base Substances 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- 239000004115 Sodium Silicate Substances 0.000 description 1
- VYKXHNKSCDJSNO-UHFFFAOYSA-N [O-]CC.[Ti+4].[O-]CC.[Ti+4] Chemical compound [O-]CC.[Ti+4].[O-]CC.[Ti+4] VYKXHNKSCDJSNO-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- WDJHALXBUFZDSR-UHFFFAOYSA-N acetoacetic acid Chemical group CC(=O)CC(O)=O WDJHALXBUFZDSR-UHFFFAOYSA-N 0.000 description 1
- HDYRYUINDGQKMC-UHFFFAOYSA-M acetyloxyaluminum;dihydrate Chemical compound O.O.CC(=O)O[Al] HDYRYUINDGQKMC-UHFFFAOYSA-M 0.000 description 1
- 239000003929 acidic solution Substances 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 125000003545 alkoxy group Chemical group 0.000 description 1
- 125000000217 alkyl group Chemical group 0.000 description 1
- 125000005233 alkylalcohol group Chemical group 0.000 description 1
- 229940009827 aluminum acetate Drugs 0.000 description 1
- 125000003277 amino group Chemical group 0.000 description 1
- 150000003868 ammonium compounds Chemical class 0.000 description 1
- 238000000149 argon plasma sintering Methods 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000002981 blocking agent Substances 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 125000003700 epoxy group Chemical group 0.000 description 1
- 125000004185 ester group Chemical group 0.000 description 1
- 239000010408 film Substances 0.000 description 1
- 150000002334 glycols Chemical class 0.000 description 1
- 150000002484 inorganic compounds Chemical class 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 150000007527 lewis bases Chemical class 0.000 description 1
- 239000003446 ligand Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- MCCIMQKMMBVWHO-UHFFFAOYSA-N octadecanoic acid;titanium Chemical compound [Ti].CCCCCCCCCCCCCCCCCC(O)=O.CCCCCCCCCCCCCCCCCC(O)=O.CCCCCCCCCCCCCCCCCC(O)=O.CCCCCCCCCCCCCCCCCC(O)=O MCCIMQKMMBVWHO-UHFFFAOYSA-N 0.000 description 1
- 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 1
- 239000003973 paint Substances 0.000 description 1
- 238000010422 painting Methods 0.000 description 1
- 239000011941 photocatalyst Substances 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 235000019353 potassium silicate Nutrition 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 235000019795 sodium metasilicate Nutrition 0.000 description 1
- 229910052911 sodium silicate Inorganic materials 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 229910000348 titanium sulfate Inorganic materials 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D1/00—Coating compositions, e.g. paints, varnishes or lacquers, based on inorganic substances
-
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82B—NANOSTRUCTURES FORMED BY MANIPULATION OF INDIVIDUAL ATOMS, MOLECULES, OR LIMITED COLLECTIONS OF ATOMS OR MOLECULES AS DISCRETE UNITS; MANUFACTURE OR TREATMENT THEREOF
- B82B3/00—Manufacture or treatment of nanostructures by manipulation of individual atoms or molecules, or limited collections of atoms or molecules as discrete units
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/36—Compounds of titanium
- C09C1/3607—Titanium dioxide
- C09C1/3684—Treatment with organo-silicon compounds
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/36—Compounds of titanium
- C09C1/3692—Combinations of treatments provided for in groups C09C1/3615 - C09C1/3684
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/84—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by UV- or VIS- data
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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- Chemical & Material Sciences (AREA)
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- Organic Chemistry (AREA)
- Nanotechnology (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
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- Condensed Matter Physics & Semiconductors (AREA)
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- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Geology (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- Wood Science & Technology (AREA)
- Manufacturing & Machinery (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Colloid Chemistry (AREA)
- Paints Or Removers (AREA)
- Catalysts (AREA)
Description
れた二酸化チタンコロイド溶液は高濃度(3〜5重量%)、且つ中性溶液である。従って、その応用分野も大いに広がり得る。
A)アルコールにチタン化合物と安定化剤を添加する工程、
B)反応溶液に撹拌しながら蒸留水を徐々に添加する工程、
C)生成した溶液に塩基性溶液を添加して中和する工程、及び
D)中和した溶液を85℃を超える温度で加熱する工程。
前記C)工程で、塩基性溶液を徐々に添加しながら生成した溶液のpHを6〜8になるように調節する。
前記D)工程で、溶液を7時間を超えて加熱後、アナターゼ構造で10nm未満のサイズの二酸化チタン微粒子が分散された中性及び透明なコロイド溶液を得ることが可能である。
(b)生成した溶液に塩基性溶液を添加することで生成した溶液を中和する工程、及び
(c)中和した溶液を75℃を超える温度で7時間を超えて加熱する工程。
。また、前記(b)工程以前に、40%四塩化チタン水溶液を全体溶液の0.01〜2重量%になるように添加するか、蒸留水を全体溶液の2〜10重量%になるように添加して加水分解反応を促進する。また、溶液を十分な時間、好ましくは1時間を超えて常温で撹拌する。(b)工程で、塩基性溶液を徐々に添加して生成した溶液のpHが6〜8になるように調節する。(c)工程で、溶液を7時間を超えて加熱後、アナターゼ構造を持ち、10nm未満のサイズの二酸化チタン微粒子が分散された中性及び透明な二酸化チタン(TiO2)コロイド溶液を得ることが可能である。
グリコールを添加する。
ルを使った二酸化チタンコロイド溶液を含むことを特徴とした、優れた透明性、付着性、結晶性、吸光度及び安定性を有する多機能性の常温硬化型コーティング剤を提供する。
7時間得られた溶液を加熱後、分散された、アナターゼ構造の二酸化チタンナノ微粒子(10nm未満)を含む、澄んでいて透明なコロイド溶液を得た。
1mlの水を使った又はアルコールを使った二酸化チタンコロイド溶液を、5mlの水又はアルコールに各々希釈した。溶液中での光散乱度を紫外/可視光分光器を使用して、410nm波長領域(光が吸収されないで散乱する一番短い波長領域)で測定した。
1mlの水を使った又はアルコールを使った二酸化チタンコロイド溶液を、5mlの水またはアルコールに各々希釈した。その溶液をガラス板表面にスピンコーティング法で塗布し、ついで、恒温槽で110℃の温度で熱処理し、その後、消しゴムで擦った。紫外/可視光分光器を用い350nmで吸光度を測定した。
1ヶ月経過後、二酸化チタンコロイド溶液の濁度の変化度を測定した。濁度は透明性と
同一の方法で測定した。
相対的な吸光度である。1mlの二酸化チタンコロイド溶液を5mlの蒸留水に希釈し、350nmの波長で吸光度を測定した。
1mlの水を使った又はアルコールを使った二酸化チタンコロイド溶液を、5mlの水又はアルコールに各々希釈した。溶液はガラス板表面にスピンコーティング法で二回塗布し、恒温槽で110℃の温度で熱処理し、その後、X線回析(XRD)を用いて薄膜の結晶性を測定した。膜が非常に薄いため、XRDは1°で実施し、2θは10°から80°の範囲で、走査速度は2°/分で測定した。
Claims (10)
- 分散された二酸化チタンナノ微粒子を含む中性及び透明な、水を使った二酸化チタンコロイド溶液を製造する方法であって、以下の工程(以下の工程において、重量%とは、生成する二酸化チタンコロイド溶液を100重量%とした場合に対する割合である)、
(A)アルコール1〜50重量%に、チタン(IV)イソプロポキシド(テトライソプロパノールチタン)、チタン(IV)ブトキシド、チタン(IV)エトキシド(チタンテトラエタノレート)、チタン(IV)メトキシド、ステアリン酸チタン(IV)、及びこれらの混合物からなる群より選択されるチタン化合物(生成する二酸化チタンコロイド溶液に分散される二酸化チタンとして換算した場合)1〜5重量%と、グリコール酸、グリコール酸塩、シュウ酸、シュウ酸塩、ペンタンジオール、ペンタンジオン、ブタンジオール、ブタンジオン、アルキルアセトアセテート、ポリエチレングリコール、水酸化セチルトリメチルアンモニウム、ポリ酢酸ビニル、ポリビニルアルコール、トリアルキルアルコールアミン((RO)3N)、及びこれらの混合物からなる群から選択される安定化剤0.1〜3重量%を添加し、溶解して反応させる工程と、
(B)前記反応した溶液に撹拌しながら蒸留水を徐々に添加する工程と、
(C)生成した溶液に、水酸化ナトリウム、アルカリ金属の塩基性化合物、アンモニア、アルキルアンモニウム基を有する塩基性化合物、アルカリ土類金属の塩基性化合物、及びアルミニウム塩基性化合物からなる群より選択される塩基性溶液を添加してpH6〜8になるようにする工程と、及び
(D)前記溶液を85℃以上の温度で加熱する工程とを含み、
前記(A)工程で、チタン化合物及び安定化剤は任意の順序で添加することが可能であることを特徴とする、分散された二酸化チタンナノ微粒子を含む中性及び透明な、水を使った二酸化チタンコロイド溶液を製造する方法。 - (A)工程で前記安定化剤の添加前およびチタン化合物をアルコールに添加した後に、前記溶液に40%四塩化チタン水溶液を添加することを特徴とする、請求項1に記載の方法。
- 前記アルコールはC1〜C4の低級アルコールからなる群から選択されることを特徴とする、請求項1又は2に記載の方法。
- (A)工程でチタン化合物に加えて、有機シリコン化合物、アルミニウム化合物、ジルコニウム化合物、鉄化合物、又はこれらの混合物をさらに添加することを特徴とする、請求項1〜3のいずれか一項に記載の方法。
- (D)工程の前記加熱手順を、高温、高圧反応器内で120℃を超える温度で5時間実施する熱水反応に置き換えることを特徴とする、請求項1〜4のいずれか一項に記載の方法。
- 分散された二酸化チタンナノ微粒子を含む中性及び透明な、アルコールを使った二酸化チタンコロイド溶液を製造する方法であって、以下の工程(以下の工程において、重量%とは、生成する二酸化チタンコロイド溶液を100重量%とした場合に対する割合である)、
(a)アルコール50〜90重量%に、チタン(IV)イソプロポキシド(テトライソプロパノールチタン)、チタン(IV)ブトキシド、チタン(IV)エトキシド(チタンテトラエタノレート)、チタン(IV)メトキシド、ステアリン酸チタン(IV)、及びこれらの混合物からなる群より選択されるチタン化合物(生成する二酸化チタンコロイド溶液に分散される二酸化チタンとして換算した場合)1〜5重量%と、グリコール酸、グリコール酸塩、シュウ酸、シュウ酸塩、ペンタンジオール、ペンタンジオン、ブタンジオール、ブタンジオン、アルキルアセトアセテート、ポリエチレングリコール、水酸化セチルトリメチルアンモニウム、ポリ酢酸ビニル、ポリビニルアルコール、トリアルキルアルコールアミン((RO)3N)、及びこれらの混合物からなる群から選択される安定化剤0.1〜3重量%を添加した後に、2〜10重量%の蒸留水を添加して反応させる工程と、(b)生成した溶液に、水酸化ナトリウム、アルカリ金属の塩基性化合物、アンモニア、アルキルアンモニウム基を有する塩基性化合物、アルカリ土類金属の塩基性化合物、及びアルミニウム塩基性化合物からなる群より選択される塩基性溶液を添加してpH6〜8になるようにする工程と、及び
(c)前記溶液を75℃以上の温度で加熱する工程とを含み、
前記(a)工程で、チタン化合物及び安定化剤は任意の順序で添加することが可能であることを特徴とする、分散された二酸化チタンナノ微粒子を含む中性及び透明な、アルコールを使った二酸化チタンコロイド溶液を製造する方法。 - (b)工程の前に、40%四塩化チタン水溶液を前記溶液にさらに添加することを特徴とする、請求項6に記載の方法。
- 前記アルコールはC1〜C4の低級アルコールからなる群から選択されることを特徴とする、請求項6又は7に記載の方法。
- (a)工程でチタン化合物に加えて、有機シリコン化合物、アルミニウム化合物、ジルコニウム化合物、鉄化合物、又はこれらの混合物をさらに添加することを特徴とする、請求項6〜8のいずれか一項に記載の方法。
- (c)工程の前記加熱手順を、高温、高圧反応器内で120℃を超える温度で5時間実施する熱水反応に置き換えることを特徴とする、請求項6〜9のいずれか一項に記載の方法。
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PCT/KR2003/001063 WO2004087578A1 (en) | 2003-04-03 | 2003-05-30 | Non-acidic, non-basic colloid solution containing dispersed titanium dioxide, method of manufacturing the same, and coating material comprising the colloid solution |
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