WO1999037582A1 - Sol colloidal d'oxyde de titane et procede de preparation associe - Google Patents
Sol colloidal d'oxyde de titane et procede de preparation associe Download PDFInfo
- Publication number
- WO1999037582A1 WO1999037582A1 PCT/JP1999/000342 JP9900342W WO9937582A1 WO 1999037582 A1 WO1999037582 A1 WO 1999037582A1 JP 9900342 W JP9900342 W JP 9900342W WO 9937582 A1 WO9937582 A1 WO 9937582A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- titanium oxide
- sol
- oxide colloid
- titanium
- weight
- Prior art date
Links
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 170
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 title claims abstract description 123
- 238000000034 method Methods 0.000 title claims description 26
- 239000002245 particle Substances 0.000 claims abstract description 60
- 239000008139 complexing agent Substances 0.000 claims abstract description 38
- 239000000126 substance Substances 0.000 claims abstract description 38
- 239000010936 titanium Substances 0.000 claims abstract description 20
- -1 amine compounds Chemical class 0.000 claims abstract description 17
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 17
- 150000001339 alkali metal compounds Chemical class 0.000 claims abstract description 4
- 239000000084 colloidal system Substances 0.000 claims description 97
- 238000004519 manufacturing process Methods 0.000 claims description 24
- 230000002378 acidificating effect Effects 0.000 claims description 23
- NQRYJNQNLNOLGT-UHFFFAOYSA-N Piperidine Chemical compound C1CCNCC1 NQRYJNQNLNOLGT-UHFFFAOYSA-N 0.000 claims description 12
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 10
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 10
- 238000002242 deionisation method Methods 0.000 claims description 7
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 claims description 6
- BCHZICNRHXRCHY-UHFFFAOYSA-N 2h-oxazine Chemical compound N1OC=CC=C1 BCHZICNRHXRCHY-UHFFFAOYSA-N 0.000 claims description 5
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 5
- 150000003868 ammonium compounds Chemical class 0.000 claims description 4
- 150000001875 compounds Chemical class 0.000 claims description 4
- 229910019142 PO4 Inorganic materials 0.000 claims description 2
- 150000003016 phosphoric acids Chemical class 0.000 claims description 2
- 150000002736 metal compounds Chemical class 0.000 claims 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims 1
- 239000010452 phosphate Substances 0.000 claims 1
- 239000011248 coating agent Substances 0.000 abstract description 25
- 238000000576 coating method Methods 0.000 abstract description 20
- 239000002253 acid Substances 0.000 abstract description 18
- 230000007935 neutral effect Effects 0.000 abstract description 14
- 239000000203 mixture Substances 0.000 abstract description 10
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical class N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 abstract description 4
- 238000001035 drying Methods 0.000 abstract description 3
- 239000000243 solution Substances 0.000 description 25
- 235000010215 titanium dioxide Nutrition 0.000 description 22
- 239000004408 titanium dioxide Substances 0.000 description 21
- 239000006185 dispersion Substances 0.000 description 19
- 230000000052 comparative effect Effects 0.000 description 16
- AEMRFAOFKBGASW-UHFFFAOYSA-N Glycolic acid Chemical compound OCC(O)=O AEMRFAOFKBGASW-UHFFFAOYSA-N 0.000 description 15
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 14
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 12
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 9
- 239000000463 material Substances 0.000 description 9
- YNAVUWVOSKDBBP-UHFFFAOYSA-N Morpholine Chemical compound C1COCCN1 YNAVUWVOSKDBBP-UHFFFAOYSA-N 0.000 description 8
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 7
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 7
- 235000011114 ammonium hydroxide Nutrition 0.000 description 7
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 description 6
- 239000002738 chelating agent Substances 0.000 description 6
- XPPKVPWEQAFLFU-UHFFFAOYSA-N diphosphoric acid Chemical compound OP(O)(=O)OP(O)(O)=O XPPKVPWEQAFLFU-UHFFFAOYSA-N 0.000 description 6
- 239000004310 lactic acid Substances 0.000 description 6
- 235000014655 lactic acid Nutrition 0.000 description 6
- 230000001699 photocatalysis Effects 0.000 description 6
- UNXRWKVEANCORM-UHFFFAOYSA-N triphosphoric acid Chemical compound OP(O)(=O)OP(O)(=O)OP(O)(O)=O UNXRWKVEANCORM-UHFFFAOYSA-N 0.000 description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 5
- 239000011247 coating layer Substances 0.000 description 5
- 238000000502 dialysis Methods 0.000 description 5
- 150000002500 ions Chemical class 0.000 description 5
- 229910052751 metal Inorganic materials 0.000 description 5
- 239000002184 metal Substances 0.000 description 5
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 4
- 241000209094 Oryza Species 0.000 description 4
- 235000007164 Oryza sativa Nutrition 0.000 description 4
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 description 4
- 229910052782 aluminium Inorganic materials 0.000 description 4
- 235000015165 citric acid Nutrition 0.000 description 4
- 230000003301 hydrolyzing effect Effects 0.000 description 4
- 239000012528 membrane Substances 0.000 description 4
- 239000003973 paint Substances 0.000 description 4
- 235000011007 phosphoric acid Nutrition 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 235000009566 rice Nutrition 0.000 description 4
- 239000011975 tartaric acid Substances 0.000 description 4
- 235000002906 tartaric acid Nutrition 0.000 description 4
- 150000003609 titanium compounds Chemical class 0.000 description 4
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 description 4
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 3
- RGHNJXZEOKUKBD-SQOUGZDYSA-N D-gluconic acid Chemical compound OC[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C(O)=O RGHNJXZEOKUKBD-SQOUGZDYSA-N 0.000 description 3
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 description 3
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 3
- 229910000831 Steel Inorganic materials 0.000 description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 3
- 150000001412 amines Chemical class 0.000 description 3
- 239000000908 ammonium hydroxide Substances 0.000 description 3
- 150000001735 carboxylic acids Chemical class 0.000 description 3
- 239000000919 ceramic Substances 0.000 description 3
- 238000009792 diffusion process Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000011156 evaluation Methods 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 230000003472 neutralizing effect Effects 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
- WRHZVMBBRYBTKZ-UHFFFAOYSA-N pyrrole-2-carboxylic acid Chemical compound OC(=O)C1=CC=CN1 WRHZVMBBRYBTKZ-UHFFFAOYSA-N 0.000 description 3
- 150000003839 salts Chemical class 0.000 description 3
- 239000010959 steel Substances 0.000 description 3
- 239000000758 substrate Substances 0.000 description 3
- 229910000348 titanium sulfate Inorganic materials 0.000 description 3
- HZAXFHJVJLSVMW-UHFFFAOYSA-N 2-Aminoethan-1-ol Chemical compound NCCO HZAXFHJVJLSVMW-UHFFFAOYSA-N 0.000 description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- RGHNJXZEOKUKBD-UHFFFAOYSA-N D-gluconic acid Natural products OCC(O)C(O)C(O)C(O)C(O)=O RGHNJXZEOKUKBD-UHFFFAOYSA-N 0.000 description 2
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 2
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 description 2
- KDYFGRWQOYBRFD-UHFFFAOYSA-N Succinic acid Natural products OC(=O)CCC(O)=O KDYFGRWQOYBRFD-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 2
- 238000005299 abrasion Methods 0.000 description 2
- 150000007513 acids Chemical class 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 150000008044 alkali metal hydroxides Chemical class 0.000 description 2
- 150000001450 anions Chemical class 0.000 description 2
- 230000000844 anti-bacterial effect Effects 0.000 description 2
- 239000002585 base Substances 0.000 description 2
- KDYFGRWQOYBRFD-NUQCWPJISA-N butanedioic acid Chemical compound O[14C](=O)CC[14C](O)=O KDYFGRWQOYBRFD-NUQCWPJISA-N 0.000 description 2
- BVKZGUZCCUSVTD-UHFFFAOYSA-N carbonic acid Chemical compound OC(O)=O BVKZGUZCCUSVTD-UHFFFAOYSA-N 0.000 description 2
- 150000001732 carboxylic acid derivatives Chemical class 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 238000005524 ceramic coating Methods 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 235000011180 diphosphates Nutrition 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 239000000174 gluconic acid Substances 0.000 description 2
- 235000012208 gluconic acid Nutrition 0.000 description 2
- 230000007062 hydrolysis Effects 0.000 description 2
- 238000006460 hydrolysis reaction Methods 0.000 description 2
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 239000003014 ion exchange membrane Substances 0.000 description 2
- 239000003456 ion exchange resin Substances 0.000 description 2
- 229920003303 ion-exchange polymer Polymers 0.000 description 2
- 239000007769 metal material Substances 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
- 229910017604 nitric acid Inorganic materials 0.000 description 2
- 239000011941 photocatalyst Substances 0.000 description 2
- 230000002265 prevention Effects 0.000 description 2
- 229940048084 pyrophosphate Drugs 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- 238000003980 solgel method Methods 0.000 description 2
- LLZRNZOLAXHGLL-UHFFFAOYSA-J titanic acid Chemical compound O[Ti](O)(O)O LLZRNZOLAXHGLL-UHFFFAOYSA-J 0.000 description 2
- 229910000349 titanium oxysulfate Inorganic materials 0.000 description 2
- 229910052725 zinc Inorganic materials 0.000 description 2
- 239000011701 zinc Substances 0.000 description 2
- POILWHVDKZOXJZ-ARJAWSKDSA-M (z)-4-oxopent-2-en-2-olate Chemical compound C\C([O-])=C\C(C)=O POILWHVDKZOXJZ-ARJAWSKDSA-M 0.000 description 1
- VILCJCGEZXAXTO-UHFFFAOYSA-N 2,2,2-tetramine Chemical compound NCCNCCNCCN VILCJCGEZXAXTO-UHFFFAOYSA-N 0.000 description 1
- RSEBUVRVKCANEP-UHFFFAOYSA-N 2-pyrroline Chemical compound C1CC=CN1 RSEBUVRVKCANEP-UHFFFAOYSA-N 0.000 description 1
- YHWMFDLNZGIJSD-UHFFFAOYSA-N 2h-1,4-oxazine Chemical compound C1OC=CN=C1 YHWMFDLNZGIJSD-UHFFFAOYSA-N 0.000 description 1
- 229910002012 Aerosil® Inorganic materials 0.000 description 1
- 229910000838 Al alloy Inorganic materials 0.000 description 1
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonium chloride Substances [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 1
- 239000004251 Ammonium lactate Substances 0.000 description 1
- 229920000298 Cellophane Polymers 0.000 description 1
- 241000195493 Cryptophyta Species 0.000 description 1
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 229920001131 Pulp (paper) Polymers 0.000 description 1
- 239000004115 Sodium Silicate Substances 0.000 description 1
- 235000021355 Stearic acid Nutrition 0.000 description 1
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- VGNJJNFWWIDONZ-UHFFFAOYSA-N acetyl acetate;titanium Chemical compound [Ti].CC(=O)OC(C)=O VGNJJNFWWIDONZ-UHFFFAOYSA-N 0.000 description 1
- 239000003929 acidic solution Substances 0.000 description 1
- 239000013543 active substance Substances 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 229910052910 alkali metal silicate Inorganic materials 0.000 description 1
- 150000001340 alkali metals Chemical class 0.000 description 1
- 239000012670 alkaline solution Substances 0.000 description 1
- 150000001408 amides Chemical class 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 229940059265 ammonium lactate Drugs 0.000 description 1
- 235000019286 ammonium lactate Nutrition 0.000 description 1
- 239000003957 anion exchange resin Substances 0.000 description 1
- RZOBLYBZQXQGFY-HSHFZTNMSA-N azanium;(2r)-2-hydroxypropanoate Chemical compound [NH4+].C[C@@H](O)C([O-])=O RZOBLYBZQXQGFY-HSHFZTNMSA-N 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 description 1
- 239000000920 calcium hydroxide Substances 0.000 description 1
- 229910001861 calcium hydroxide Inorganic materials 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000003729 cation exchange resin Substances 0.000 description 1
- 239000013522 chelant Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- XFVGXQSSXWIWIO-UHFFFAOYSA-N chloro hypochlorite;titanium Chemical compound [Ti].ClOCl XFVGXQSSXWIWIO-UHFFFAOYSA-N 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000001877 deodorizing effect Effects 0.000 description 1
- 235000014113 dietary fatty acids Nutrition 0.000 description 1
- 239000003085 diluting agent Substances 0.000 description 1
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 238000002845 discoloration Methods 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 229910052571 earthenware Inorganic materials 0.000 description 1
- 238000000909 electrodialysis Methods 0.000 description 1
- RLGKNOKKEQLVIU-UHFFFAOYSA-N ethanol Chemical compound CCO.CCO.CCO.CCO RLGKNOKKEQLVIU-UHFFFAOYSA-N 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 239000000194 fatty acid Substances 0.000 description 1
- 229930195729 fatty acid Natural products 0.000 description 1
- 230000004133 fatty acid degradation Effects 0.000 description 1
- 150000004665 fatty acids Chemical class 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- ZZUFCTLCJUWOSV-UHFFFAOYSA-N furosemide Chemical compound C1=C(Cl)C(S(=O)(=O)N)=CC(C(O)=O)=C1NCC1=CC=CO1 ZZUFCTLCJUWOSV-UHFFFAOYSA-N 0.000 description 1
- 230000009931 harmful effect Effects 0.000 description 1
- 238000010335 hydrothermal treatment Methods 0.000 description 1
- 230000000640 hydroxylating effect Effects 0.000 description 1
- 230000001678 irradiating effect Effects 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- FUJCRWPEOMXPAD-UHFFFAOYSA-N lithium oxide Chemical compound [Li+].[Li+].[O-2] FUJCRWPEOMXPAD-UHFFFAOYSA-N 0.000 description 1
- 229910001947 lithium oxide Inorganic materials 0.000 description 1
- 230000000873 masking effect Effects 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- UIUXUFNYAYAMOE-UHFFFAOYSA-N methylsilane Chemical compound [SiH3]C UIUXUFNYAYAMOE-UHFFFAOYSA-N 0.000 description 1
- 235000016337 monopotassium tartrate Nutrition 0.000 description 1
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 1
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 239000011368 organic material Substances 0.000 description 1
- 235000006408 oxalic acid Nutrition 0.000 description 1
- 150000004893 oxazines Chemical class 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical class [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 description 1
- BAQNULZQXCKSQW-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[O-2].[O-2].[Ti+4].[Ti+4] BAQNULZQXCKSQW-UHFFFAOYSA-N 0.000 description 1
- 235000021317 phosphate Nutrition 0.000 description 1
- 150000003013 phosphoric acid derivatives Chemical class 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 229920000768 polyamine Polymers 0.000 description 1
- 229920006267 polyester film Polymers 0.000 description 1
- KYKNRZGSIGMXFH-ZVGUSBNCSA-M potassium bitartrate Chemical compound [K+].OC(=O)[C@H](O)[C@@H](O)C([O-])=O KYKNRZGSIGMXFH-ZVGUSBNCSA-M 0.000 description 1
- 229940086065 potassium hydrogentartrate Drugs 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 description 1
- 229940005657 pyrophosphoric acid Drugs 0.000 description 1
- ZVJHJDDKYZXRJI-UHFFFAOYSA-N pyrroline Natural products C1CC=NC1 ZVJHJDDKYZXRJI-UHFFFAOYSA-N 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 150000004756 silanes Chemical class 0.000 description 1
- 229920002050 silicone resin Polymers 0.000 description 1
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 1
- 229910052911 sodium silicate Inorganic materials 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000008117 stearic acid Substances 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- VKFFEYLSKIYTSJ-UHFFFAOYSA-N tetraazanium;phosphonato phosphate Chemical compound [NH4+].[NH4+].[NH4+].[NH4+].[O-]P([O-])(=O)OP([O-])([O-])=O VKFFEYLSKIYTSJ-UHFFFAOYSA-N 0.000 description 1
- CBXCPBUEXACCNR-UHFFFAOYSA-N tetraethylammonium Chemical compound CC[N+](CC)(CC)CC CBXCPBUEXACCNR-UHFFFAOYSA-N 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- 150000003573 thiols Chemical class 0.000 description 1
- 150000003608 titanium Chemical class 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 238000003911 water pollution Methods 0.000 description 1
- 239000003021 water soluble solvent Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
- C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
- C23C18/1204—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material inorganic material, e.g. non-oxide and non-metallic such as sulfides, nitrides based compounds
- C23C18/1208—Oxides, e.g. ceramics
- C23C18/1216—Metal oxides
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- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/04—Oxides; Hydroxides
- C01G23/047—Titanium dioxide
- C01G23/08—Drying; Calcining ; After treatment of titanium oxide
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- 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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
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- C01G23/04—Oxides; Hydroxides
- C01G23/047—Titanium dioxide
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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
- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/22—Surface treatment of glass, not in the form of fibres or filaments, by coating with other inorganic material
- C03C17/23—Oxides
- C03C17/25—Oxides by deposition from the liquid phase
- C03C17/256—Coating containing TiO2
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
- C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
- C23C18/125—Process of deposition of the inorganic material
- C23C18/1262—Process of deposition of the inorganic material involving particles, e.g. carbon nanotubes [CNT], flakes
- C23C18/127—Preformed particles
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
- C01P2004/82—Particles consisting of a mixture of two or more inorganic phases two phases having the same anion, e.g. both oxidic phases
- C01P2004/84—Particles consisting of a mixture of two or more inorganic phases two phases having the same anion, e.g. both oxidic phases one phase coated with the other
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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
- C03C2217/00—Coatings on glass
- C03C2217/20—Materials for coating a single layer on glass
- C03C2217/21—Oxides
- C03C2217/212—TiO2
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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
- C03C2217/00—Coatings on glass
- C03C2217/70—Properties of coatings
- C03C2217/71—Photocatalytic coatings
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- 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
- C03C2218/00—Methods for coating glass
- C03C2218/10—Deposition methods
- C03C2218/11—Deposition methods from solutions or suspensions
- C03C2218/113—Deposition methods from solutions or suspensions by sol-gel processes
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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
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/46—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on titanium oxides or titanates
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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
- C04B35/63—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 using additives specially adapted for forming the products, e.g.. binder binders
- C04B35/632—Organic additives
Definitions
- the present invention relates to a titanium oxide colloid sol and a method for producing the same. More specifically, the present invention relates to a colloid sol of titanium dioxide mainly used as a semiconductor photocatalyst and a method for producing the same.
- the titanium oxide colloid sol of the present invention can be used as a raw material for various functional coating agents such as ultraviolet absorption, stain prevention, hydrophilicity, antifogging, antibacterial, deodorizing, and water treatment. Background art
- ceramic coatings that have better heat resistance and abrasion resistance than organic coatings include alkali metal silicates, phosphates, silica sols, and metals.
- Oxide-based paints are known o
- titanium oxide can exhibit an excellent photocatalytic effect, and when irradiated with ultraviolet light, exhibits high oxidizing power
- titanium oxide which has excellent photocatalytic activity, is present on the surface of an object to be coated such as metal, glass, and ceramic to prevent adhesion of dirt, decompose odorous components, purify water, and prevent water pollution.
- antibacterial, prevention of algae reproduction PT / JP99 / 00342 is known to be effective in promoting the decomposition of hard-to-decompose waste
- the most common method of forming a titanium oxide film is a method of applying a hydrolyzed titanium alkoxide, that is, a sol-gel method.
- a method of adding amide or glycol to a titanium alkoxide As described above, a method of adding an alcohol amine to a titanium alkoxide is known.
- titanium oxide fine particles crystallized by hydrothermal treatment are disclosed. Is dispersed in an acid solution having a pH of 3 or less, and a method of applying the dispersion is known.
- the above-mentioned sol-gel method and the method of peptizing or dispersing with an acid have a serious problem that, since the colloid solution is acidic, when applied to the surface of metal, paper, or the like, these materials corrode or deteriorate. It was hot.
- coating equipment such as coaters, printing machines and spray guns may be corroded, and the coating work environment for workers may deteriorate. It was known.
- An object of the present invention is to solve the above-mentioned problems of the conventional titanium oxide photocatalyst solution, to be stable even under neutral conditions, to be able to perform a coating operation safely, and to be able to dry at room temperature.
- An object of the present invention is to provide a titanium oxide colloid sol capable of forming a colorless and transparent film and a method for producing the same.
- the above object can be achieved by the following titanium oxide sol of the present invention and a method for producing the same.
- the titanium oxide colloid sol of the present invention comprises 50 to 100 parts by weight of negatively charged titanium oxide colloid particles, 5 to 50 parts by weight of a complexing agent, and 1 to 50 parts by weight. Alkali substances.
- the titanium oxide sol of the present invention has a pH of 5-10.
- the production method (1) of the titanium oxide colloid sol of the present invention comprises the steps of: adding 50 to 100 parts by weight of titanium oxide colloid particles and 5 to 50 parts by weight of an acidic titanium oxide colloid sol containing a complexing agent; The pH value of the sol solution is adjusted to 5 to 10 by adding an active substance, whereby the titanium oxide particles are negatively charged.
- the method (2) for producing a titanium oxide colloid sol according to the present invention comprises: adding an acidic titanium oxide sol containing 50 to 100 parts by weight of titanium oxide colloid particles and 50 to 50 parts by weight of a complexing agent; The pH of the sol solution is adjusted to 6 to 12 by adding a neutralizing substance, and the sol solution is further subjected to deionization treatment, whereby the titanium oxide colloid particles are negatively charged. Is included. BEST MODE FOR CARRYING OUT THE INVENTION
- the present inventors firstly react an inorganic titanium salt or titanium alkoxide such as titanium chloride and titanium sulfate with water in an acidic manner to prepare a titanium dioxide colloid solution.
- the charging behavior of the acidic colloid sol of titanium was analyzed.
- the oxidized titanium colloid particles have a stable positive charge in an acidic state, but when this is neutralized with an alkaline solution, when the pH is in the range of 3 to 5, the titanium oxidized titanium colloid particles are neutralized.
- the colloid particles lose almost no charge, and the colloid particles become extremely unstable.They are strongly agglomerated and difficult to re-disperse, and when the alkalinity is further increased, the aggregated titanium oxide titanium colloid particles are negatively charged. It was confirmed that.
- the present inventors have repeatedly studied a method for providing titanium oxide colloid particles with stable charge and good dispersibility even in a neutral region.o
- titanium oxide colloid particles are strongly agglomerated even if the pH of the sol solution is adjusted to an alkaline range by adding an alkali metal hydroxide or an aqueous ammonia solution to the titanium oxide acidic colloid sol solution. then becomes redispersion impossible, want earthenware pots phenomenon observed in a slide Li one shaped suspension, the cause of this phenomenon, the water T i 4 + ions present in the sol liquid is colloidal form.
- condensed phosphorus such as polyvalent carboxylic acid, hydroxycarboxylic acid, and oxalic acid capable of forming a complex with Ti "ion in an acidic titanium oxide colloid sol in advance.
- Complexing agents selected from acids etc. JP99 / 00342
- an alkali component such as ammonia water and morpholine is added to increase the pH of the colloid sol solution to a desired value.
- the titanium oxide colloid particles can be negatively charged by adjusting the pH, and the titanium oxide colloid sol can be dispersed stably due to the negative charge of the titanium oxide colloid particles in the neutral to alkaline pH range. It has been found that a colorless and transparent titanium dioxide film having excellent adhesion can be obtained even by drying at room temperature by applying the sol to the object to be treated.
- a composition of the titanium oxide sol a neutral sol containing a negatively charged titanium oxide particle component, the complexing agent, and an alkaline component has good stability and dispersibility. However, it has been found that the above-mentioned desired performance is satisfied.
- the titanium oxide sol of the present invention contains 50 to 100 parts by weight of titanium oxide colloid particles, and the titanium oxide colloid particles are negatively charged in the neutral sol solution. ing. If the titanium oxide colloid particles are positively charged in the neutral region, the dispersion of the colloid particles becomes unstable. The sign of the charge of the particles can be easily known by a zeta potential measuring device or the like.
- titanium oxide used in the present invention include anatase-type titanium dioxide (including metatitanic acid), orthotitanic acid and rutile. Although other titanium dioxides such as thiol type can be used, among these, anatase type titanium dioxide (including metatitanic acid) and orthotitanic acid are most preferably used.
- the particle size of the titanium oxide colloid particles is not particularly limited, but is generally preferably from 1 nm to 500 nm, more preferably from 3 to 120 nm.
- the titanium dioxide colloid particles are obtained by dissolving at least one kind of inorganic titanium compounds such as titanium chloride, titanium oxychloride, titanium sulfate and titanyl sulfate in water, and adding hydrochloric acid or It is obtained by adding nitric acid etc. as a catalyst and hydrolyzing at room temperature or by heating.
- a method for hydrolyzing an organic titanium compound such as titanium alkoxide or titanium acetyl acetate can be used.
- the titanium oxide colloid particles formed in the acidic solution by the above method are positively charged, when the alkaline component is added to this sol solution to adjust the pH of the sol solution to 6 or more, However, it is necessary to negatively charge the titanium dioxide particles by adding a complexing agent to the sol.
- the titanium oxide sol of the present invention contains a complexing agent in a proportion of 5 to 50 parts by weight.
- the complexing agent that can be used in the present invention includes a chelating compound.
- the chelating compound preferably has at least one carboxyl group in its molecular skeleton. Those having a strong chelating effect on Ti 4 + ions are preferred.
- Preferred chelating compounds are polyvalent carboxylic acids and hydroxycarboxylic acids such as gluconic acid, glycolic acid, lactic acid, tartaric acid, citric acid, lingic acid and succinic acid, as well as condensed phosphoric acid,
- the most preferred complexing agent is the above-mentioned condensed phosphoric acid, especially pyrroline Acid and tripolyphosphoric acid.
- the titanium oxide colloid sol of the present invention needs to contain 1 to 50 parts by weight of an alkaline substance in addition to the complexing agent, and the sol solution has a pH of 5 to 9 It is preferable that it is adjusted to the range of.
- the alkaline substance is effective for neutralizing acidic ions such as hydrochloric acid ions or sulfate ions remaining in the sol solution, and for giving a stable negative charge to titanium dioxide particles.
- the alkaline substance used in the titanium oxide colloid sol of the present invention preferably contains at least one selected from an ammonium compound, an alkali metal compound, and an amine.
- Ammonia (ammonia water), sodium hydroxide, sodium hydroxide, lithium hydroxide, sodium silicate, and polyamines such as ethylenediamine and triethylenetetrathamine Etc. can be used.
- oxazines such as morpholine, piperidine, and colin can be used.
- oxazine, piperidine, ammonium hydroxide, and triethanol ethanol are easily volatilized from the coating layer. It is preferable to use a low molecular weight amine such as mine.
- both of the complexing agent and the alkaline substance are combined, such as, for example, ammonium pyrophosphate, ammonium lactate, and potassium hydrogen tartrate. May be used.
- the other components contained in the titanium oxide colloid sol of the present invention may include chloride ion, sulfate ion, and / or alcohol derived from the used titanium raw material. Consists essentially of water.
- the titanium dioxide colloid sol of the present invention is coated When used as a coating agent, it is also preferable to replace a part of water with a water-soluble solvent such as alcohol, glycol or ketone as an auxiliary solvent. In this case, it is also possible to improve the physical properties of the coating film by adding a silica derivative such as silica sol-alkyltrimethoxysilane as a binder.
- the weight ratio of the complexing agent to the weight of the titanium oxide colloid particles is too small, the dispersion of the colloid particles becomes insufficient, and a stable sol may be obtained. Can not. If the weight ratio of the complexing agent is too large, the hardness of the obtained coating film is unpreferably reduced. If the proportion of the alkaline substance is too large, the hardness of the coating film decreases, or the composition is not preferable because it shows corrosiveness to metals such as aluminum and zinc. However, it is not preferable because the sol solution becomes acidic.
- the acidic titanium oxide sol containing 50 to 100 parts by weight of titanium oxide colloid particles and 50 to 50 parts by weight of a complexing agent is added to the titanium oxide colloid sol.
- a lipophilic substance is added to adjust the pH of the sol to 5 to 10, thereby negatively charging titanium oxide colloid particles.
- the acidic titanium oxide sol used in the method (1) or (2) of the present invention comprises at least one inorganic titanium compound selected from titanium chloride, oxytitanium chloride, titanium sulfate and titanyl sulfate. It is obtained by dissolving in water, adding a catalyst consisting of hydrochloric acid and / or nitric acid as needed, and hydrolyzing at room temperature or by heating. Alternatively, titanium oxide colloid particles can also be obtained by hydrolyzing an organic titanium compound such as titanium alkoxide or titanium dimethyl acetylacetonate.
- the complexing agent used in the methods (1) and (2) of the present invention is preferably 99/00342
- Examples of the aluminum substance that can be used in the production methods (1) and (2) of the titanium oxide sol of the present invention include ammonium compounds such as ammonium hydroxide, amines such as ethanolamine, and morpholine. It is preferable to use oxazine, piperidine, colin, etc.
- alkali metal hydroxides are relatively unfavorable.
- the amount of the alkaline substance added is such that the pH of the sol is in the range of 5-10. The addition of the alkaline substance causes the titanium dioxide particles in the titanium oxide colloid to be negatively charged.
- a mixture of titanium dioxide colloid particles and a complexing agent is further mixed with a silane derivative such as epoxysilane or methylsilane.
- a hydrolysis product or a partial hydrolysis product thereof the charge of the titanium oxide colloid particles obtained by the addition of the alkaline substance is further stabilized, and when this is used as a coating agent, Coatability can also be improved o
- the titanium oxide colloid particles and the complexing agent used in the production method (2) of the present invention are the same as the titanium oxide colloid particles and the complexing agent used in the production method (1) of the present invention. Can be used.
- the alkaline substance used in the production method (2) of the present invention the same alkaline substance used in the aforementioned method (1) of the present invention can be used. Um, hydroxylating room and water The use of an alkali metal compound such as lithium oxide is also preferred.
- the alkaline substance preferably has a pH of the sol solution of 6 to 12, preferably? It is added in an amount necessary to raise to ⁇ 9. If the pH of the sol after addition of the alkaline substance is less than 6, the dispersion of the coide particles becomes insufficient, and if the pH of the sol exceeds 12 the obtained titanium oxide colloid sol is It is not preferred because it shows strong corrosiveness to metallic materials in contact with it.
- the sol is subjected to a deionization treatment to remove excess ions in the sol.
- the pH of the titanium oxide colloid sol is between 5 and 9 and more preferably between 6 and 8.5 by deionization.
- the amount of application is adjusted so that the amount of titanium dioxide adhered is 200 to 200 g / m 2.
- the coating layer can be dried not only by heating but also at room temperature.
- an organic compound such as carboxylic acid is used as the complexing agent and is dried at a temperature of 100 ° C. or less, a wavelength of 4 nm is applied to the obtained coating layer during or after the coating layer is dried. It is preferable to decompose the complexing agent by irradiating ultraviolet rays having a wavelength of less than 100 nm.
- the negatively charged titanium oxide colloid sol of the present invention has a carboxyl group.
- a complexing agent containing a chelating compound and / or a condensed phosphoric acid or a salt thereof converts tetravalent titan ions remaining as unreacted components into a conventional acidic titanium oxide sol.
- Masking, thereby preventing the titanium oxide colloid particles from gelling and precipitating in the neutral region, and the negative charge charged to the complexing agent adsorbed on the titanium oxide colloid particles causes positively charged titanium oxide It has the effect of neutralizing the colloid particles and further negatively charging them, so that a stable neutral titanium oxide sol can be obtained.
- the organic chelating agent contained therein is decomposed into water and carbon dioxide gas by the photocatalytic effect of titanium dioxide, and therefore has no harmful effect.
- the negatively charged titanium oxide colloid sol of the present invention which is neutralized by the addition of an alkaline substance such as oxazine and piperidine, can completely turn the titanium oxide colloid sol into a neutral sol, It can be produced by adding the above-mentioned alkaline component to an acidic titanium oxide sol containing a complexing agent.
- deionization treatment is performed by a method such as dialysis using a semipermeable membrane.
- Comparative Example 1 In Comparative Example 1, Comparative Example 2, Examples 1 to 7, Example 12, Example 14, and Examples 16 to 18, prepared as titanium oxide colloid by the following method. The one that was used was used.
- An aqueous titanium chloride solution (Ti : 15 to 16% by weight) manufactured by Sumitomo Chemical Co., Ltd. is diluted with water and deionized with an ion-exchange membrane to prepare an aqueous oxytitanium chloride solution.
- the mixture was heated to a temperature of 70 to 85 ° C. and hydrolyzed to obtain a titanium dioxide colloid sol having ⁇ 1-2.
- the diameter of the titanium dioxide crystal particles measured by a transmission electron microscope was 0.002 to 0.01 ⁇ m.
- the dry weight concentration of titanium oxide colloid particles in this colloid sol was 5.0%.
- the complexing agents are listed in Tables 1 and 2 from dalconic acid, glycolic acid, lactic acid, tartaric acid, citric acid, lingoic acid, pyrrolic acid, and tripoliric acid. Selected and used as shown. For these chemicals, first-class reagents manufactured by Wako Pure Chemical Industries, Ltd. were used.
- Ammonia water (ammonium hydroxide), sodium hydroxide, calcium hydroxide, lithium hydroxide, triethanolamine, triethylenetetramine, morpholine (tetraethylamine) Hydro 1, 4 —oxazine Table 1 and Table 2 were used by selecting from among, pyridine, and coli. These chemicals used reagent grade 1 or equivalent o
- Tables 1 and 2 show the compositions of the titanium oxide sols used in Comparative Examples and Examples.
- the positive and negative charges of the titanium oxide particles were measured for the obtained sol using a zeta potential measuring device.
- Example 1 Example 1, Example 5, Example 7, Example 8, Example 13 and Example 17, an aluminum alloy was used as the base material.
- acid paper was used.
- Comparative Examples 3, 2, 11, and 12 zinc-plated steel sheets were used, and Comparative Examples 4 and 5 were used.
- steel sheets were used, and in Examples 14 and 16, stainless steel sheets (SUS304) were used.
- SUS304 stainless steel sheets
- the acidic sol A) or B) was used as a raw material titanium oxide sol.
- the pH of the sol was adjusted from 7 to 8 by adding an alkaline substance without adding a complexing agent.
- Comparative Example 2 Comparative Example 4, Examples 1 to 4, Examples 8 to 9, and Examples 12 to 15, a complexing agent was added to the acidic sol, and then the alkaline substance was added. Was added to adjust the pH value to the pH value shown in Table 1, respectively.
- Comparative Example 3 Examples 5 to 7, and Examples 10 to 11, acidic sols A) or B) were used, and a complexing agent was added thereto to further increase the alkalinity. The substance was added until the pH of the sol became 6 to 12 to disperse the titanium oxide particles.
- the obtained titanium oxide colloid sol solution was deionized using a semipermeable membrane (cellophane membrane). Diffusion dialysis was performed for 24 hours in distilled water. In Examples 7, 11, and 18, the sol was passed through a column containing an anion-exchange resin and a cation-exchange resin instead of diffusion dialysis, and deionized. Was given.
- adhesion of the coating film was judged to be good, slightly poor, and poor according to the JIS-K 5500 cross-cut tape method coating adhesion test.
- the coating film was drawn with a JIS-K5400 pencil scratch test pencil, and the hardness was measured by pencil hardness. (Evaluation of substrates other than paper) (Photocatalytic activity)
- Stearic acid was diluted in ethanol and applied to the test piece, which was applied and dried on the test piece.
- the test piece was irradiated with ultraviolet light for 24 hours with a 20 W black client, and the difference between the weights before and after irradiation was 24 hours.
- Fatty acid degradation rate per unit (unit: mg / m 2 ⁇ day) was determined.
- titanium oxide colloid sols of Examples 1 to 18 and Comparative Examples 1 to 4 The composition and coating performance are shown in Table 1 and Table 2.
- Example 1 V ⁇ U «JA ⁇ J scattering ⁇ good good H 230 good 7 n gel tight fc3 ⁇ no 18 8 no J HA good good H 210 room experiment 3 qn citric acid (40) Q 7 R Sword ⁇ Auto Good 240
- Example 4 55 Tartaric acid (25) 3 5.2 Dispersion good H 220 J Li 80 Rinyu (8) 1 5 8.2 Dispersion rice cake good 2 H 21 0
- Difficult 6 70 Lactic acid (1 0) 6 7.0 Good Dispersion Good Good 280
- the conventional titanium oxide sol or the titanium oxide sols of Comparative Examples 1 to 4 produced by the production method can provide satisfactory coating performance for materials that are easily corroded or deteriorated. I could't. According to the titanium oxide sol and the method for producing a titanium oxide sol of Examples 1 to 18 according to the present invention, good coating performance was obtained in each case. Industrial applicability
- the titanium oxide colloid sol of the present invention can be applied to a substrate that has been conventionally difficult to use, such as a corrosive metal material or an easily deteriorated organic material.
- Neutral photocatalytic titanium oxide sol with stable and good dispersibility that can be used as a coating agent.
- This titanium oxide colloid sol can be used to decompose dirt, absorb ultraviolet light, sterilize, decompose gas, When applied to various purposes such as water purification, it can be applied to a wide range of materials, solving problems in the working environment and safety. Therefore, the titanium oxide colloid sol of the present invention and the method for producing the same have practically high value.
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Description
Claims
Priority Applications (3)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US09/601,034 US6420437B1 (en) | 1998-01-27 | 1999-01-27 | Titanium oxide colloidal sol and process for the preparation thereof |
EP99901886A EP1052225B1 (en) | 1998-01-27 | 1999-01-27 | Titanium oxide colloidal sol and process for the preparation thereof |
DE69920172T DE69920172T2 (de) | 1998-01-27 | 1999-01-27 | Kolloidales Titandioxidsol und Verfahren zur Herstellung desselben |
Applications Claiming Priority (4)
Application Number | Priority Date | Filing Date | Title |
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JP10/13811 | 1998-01-27 | ||
JP1381198 | 1998-01-27 | ||
JP10282938A JP3080162B2 (ja) | 1998-01-27 | 1998-10-05 | 酸化チタンゾルおよびその製造方法 |
JP10/282938 | 1998-10-05 |
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WO1999037582A1 true WO1999037582A1 (fr) | 1999-07-29 |
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PCT/JP1999/000342 WO1999037582A1 (fr) | 1998-01-27 | 1999-01-27 | Sol colloidal d'oxyde de titane et procede de preparation associe |
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US (1) | US6420437B1 (ja) |
EP (1) | EP1052225B1 (ja) |
JP (1) | JP3080162B2 (ja) |
KR (1) | KR100562173B1 (ja) |
DE (1) | DE69920172T2 (ja) |
TW (1) | TW443992B (ja) |
WO (1) | WO1999037582A1 (ja) |
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- 1999-01-27 DE DE69920172T patent/DE69920172T2/de not_active Expired - Lifetime
- 1999-01-27 EP EP99901886A patent/EP1052225B1/en not_active Expired - Lifetime
- 1999-01-27 KR KR1020007008173A patent/KR100562173B1/ko not_active IP Right Cessation
- 1999-01-27 US US09/601,034 patent/US6420437B1/en not_active Expired - Fee Related
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2002038682A1 (fr) * | 2000-11-10 | 2002-05-16 | Rhodia Chimie | Dispersion aqueuse de dioxyde de titane, substrat obtenu a partir de cette dispersion et procede d'autonettoyage dudit substrat |
FR2816610A1 (fr) * | 2000-11-10 | 2002-05-17 | Rhodia Chimie Sa | Dispersion aqueuse de dioxyde de titane, substrat obtenu a partir de cette dispersion et procede d'autonettoyage dudit substrat |
US20120128604A1 (en) * | 2001-08-10 | 2012-05-24 | Nihonkoken Kougyo Kabushiki Kaisha | Method for Manufacturing Highly Iridescent Titanium Oxide Composition |
KR20010099352A (ko) * | 2001-09-21 | 2001-11-09 | 최명식 | 광촉매 도료가 코팅된 자동차 유리 |
Also Published As
Publication number | Publication date |
---|---|
EP1052225B1 (en) | 2004-09-15 |
TW443992B (en) | 2001-07-01 |
DE69920172T2 (de) | 2005-01-27 |
EP1052225A1 (en) | 2000-11-15 |
JPH11278843A (ja) | 1999-10-12 |
JP3080162B2 (ja) | 2000-08-21 |
DE69920172D1 (de) | 2004-10-21 |
KR100562173B1 (ko) | 2006-03-20 |
KR20010034407A (ko) | 2001-04-25 |
EP1052225A4 (en) | 2002-01-30 |
US6420437B1 (en) | 2002-07-16 |
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