JP6352527B2 - 光触媒機能性フィルム及びこの製造方法 - Google Patents
光触媒機能性フィルム及びこの製造方法 Download PDFInfo
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- JP6352527B2 JP6352527B2 JP2017506658A JP2017506658A JP6352527B2 JP 6352527 B2 JP6352527 B2 JP 6352527B2 JP 2017506658 A JP2017506658 A JP 2017506658A JP 2017506658 A JP2017506658 A JP 2017506658A JP 6352527 B2 JP6352527 B2 JP 6352527B2
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- Prior art keywords
- tio
- visible light
- functional film
- photocatalytic
- amorphous
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- 230000001699 photocatalysis Effects 0.000 title claims description 63
- 238000004519 manufacturing process Methods 0.000 title claims description 14
- 239000011941 photocatalyst Substances 0.000 claims description 82
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 78
- 239000002245 particle Substances 0.000 claims description 61
- 230000004888 barrier function Effects 0.000 claims description 36
- 239000000463 material Substances 0.000 claims description 36
- 239000003795 chemical substances by application Substances 0.000 claims description 33
- 229910044991 metal oxide Inorganic materials 0.000 claims description 23
- 150000004706 metal oxides Chemical class 0.000 claims description 23
- 229910052751 metal Inorganic materials 0.000 claims description 22
- 239000002184 metal Substances 0.000 claims description 22
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 19
- 230000000694 effects Effects 0.000 claims description 19
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 12
- 239000000758 substrate Substances 0.000 claims description 12
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 10
- 239000002904 solvent Substances 0.000 claims description 10
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 9
- 239000002253 acid Substances 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 9
- 239000002243 precursor Substances 0.000 claims description 9
- 230000018044 dehydration Effects 0.000 claims description 8
- 238000006297 dehydration reaction Methods 0.000 claims description 8
- 239000010936 titanium Substances 0.000 claims description 8
- 229910052719 titanium Inorganic materials 0.000 claims description 8
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 7
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 6
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 6
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 6
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 6
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- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 3
- 229910052684 Cerium Inorganic materials 0.000 claims description 3
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 3
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 3
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 3
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 3
- 229910052788 barium Inorganic materials 0.000 claims description 3
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 claims description 3
- 229910052793 cadmium Inorganic materials 0.000 claims description 3
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 claims description 3
- 229910052791 calcium Inorganic materials 0.000 claims description 3
- 239000011575 calcium Substances 0.000 claims description 3
- 229910052804 chromium Inorganic materials 0.000 claims description 3
- 239000011651 chromium Substances 0.000 claims description 3
- 229910017052 cobalt Inorganic materials 0.000 claims description 3
- 239000010941 cobalt Substances 0.000 claims description 3
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 3
- 229910052802 copper Inorganic materials 0.000 claims description 3
- 239000010949 copper Substances 0.000 claims description 3
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 3
- 229910052737 gold Inorganic materials 0.000 claims description 3
- 239000010931 gold Substances 0.000 claims description 3
- 229910052742 iron Inorganic materials 0.000 claims description 3
- 229910052749 magnesium Inorganic materials 0.000 claims description 3
- 239000011777 magnesium Substances 0.000 claims description 3
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 claims description 3
- 229910052750 molybdenum Inorganic materials 0.000 claims description 3
- 239000011733 molybdenum Substances 0.000 claims description 3
- 229910052759 nickel Inorganic materials 0.000 claims description 3
- 229910000484 niobium oxide Inorganic materials 0.000 claims description 3
- URLJKFSTXLNXLG-UHFFFAOYSA-N niobium(5+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Nb+5].[Nb+5] URLJKFSTXLNXLG-UHFFFAOYSA-N 0.000 claims description 3
- QGLKJKCYBOYXKC-UHFFFAOYSA-N nonaoxidotritungsten Chemical compound O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1 QGLKJKCYBOYXKC-UHFFFAOYSA-N 0.000 claims description 3
- 229910052697 platinum Inorganic materials 0.000 claims description 3
- 229910052705 radium Inorganic materials 0.000 claims description 3
- HCWPIIXVSYCSAN-UHFFFAOYSA-N radium atom Chemical compound [Ra] HCWPIIXVSYCSAN-UHFFFAOYSA-N 0.000 claims description 3
- 229910052712 strontium Inorganic materials 0.000 claims description 3
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 claims description 3
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 3
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims description 3
- 229910052721 tungsten Inorganic materials 0.000 claims description 3
- 239000010937 tungsten Substances 0.000 claims description 3
- 229910001930 tungsten oxide Inorganic materials 0.000 claims description 3
- 229910052720 vanadium Inorganic materials 0.000 claims description 3
- 229910052725 zinc Inorganic materials 0.000 claims description 3
- 239000011701 zinc Substances 0.000 claims description 3
- 239000011787 zinc oxide Substances 0.000 claims description 3
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 claims 1
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 claims 1
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 18
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- 230000000052 comparative effect Effects 0.000 description 10
- 239000000126 substance Substances 0.000 description 7
- 238000000354 decomposition reaction Methods 0.000 description 6
- 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 description 6
- 229920002799 BoPET Polymers 0.000 description 5
- 239000000243 solution Substances 0.000 description 5
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- AFCARXCZXQIEQB-UHFFFAOYSA-N N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CCNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 AFCARXCZXQIEQB-UHFFFAOYSA-N 0.000 description 3
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 3
- 230000000844 anti-bacterial effect Effects 0.000 description 3
- 238000004332 deodorization Methods 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- 229910017604 nitric acid Inorganic materials 0.000 description 3
- -1 superoxide anions Chemical class 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- HORQAOAYAYGIBM-UHFFFAOYSA-N 2,4-dinitrophenylhydrazine Chemical compound NNC1=CC=C([N+]([O-])=O)C=C1[N+]([O-])=O HORQAOAYAYGIBM-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- ZMIGMASIKSOYAM-UHFFFAOYSA-N cerium Chemical compound [Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce] ZMIGMASIKSOYAM-UHFFFAOYSA-N 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 239000008199 coating composition Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 125000000524 functional group Chemical group 0.000 description 2
- 238000004128 high performance liquid chromatography Methods 0.000 description 2
- 238000006460 hydrolysis reaction Methods 0.000 description 2
- 239000002923 metal particle Substances 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 238000007086 side reaction Methods 0.000 description 2
- 238000006557 surface reaction Methods 0.000 description 2
- GPPXJZIENCGNKB-UHFFFAOYSA-N vanadium Chemical compound [V]#[V] GPPXJZIENCGNKB-UHFFFAOYSA-N 0.000 description 2
- 239000003377 acid catalyst Substances 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
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- 125000003158 alcohol group Chemical group 0.000 description 1
- 150000004703 alkoxides Chemical class 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- YHWCPXVTRSHPNY-UHFFFAOYSA-N butan-1-olate;titanium(4+) Chemical compound [Ti+4].CCCC[O-].CCCC[O-].CCCC[O-].CCCC[O-] YHWCPXVTRSHPNY-UHFFFAOYSA-N 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 239000003256 environmental substance Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
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- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 238000013032 photocatalytic reaction Methods 0.000 description 1
- 238000012643 polycondensation polymerization Methods 0.000 description 1
- 239000010970 precious metal Substances 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 238000003756 stirring Methods 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
- 229910052723 transition metal Inorganic materials 0.000 description 1
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Classifications
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- B01J21/06—Silicon, titanium, zirconium or hafnium; Oxides or hydroxides thereof
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- B01J23/682—Silver or gold with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium with vanadium, niobium, tantalum or polonium
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- B01J23/683—Silver or gold with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium with chromium, molybdenum or tungsten
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Description
本発明の一具体例において、基材層、バリアー層、及び光触媒層の積層構造で、前記バリアー層は非結晶性TiO2膜であり、前記光触媒層は非結晶性TiO2膜;及び前記非結晶性TiO2膜の表面に形成された可視光活性光触媒剤粒子を含む光触媒機能性フィルムを提供する。
媒剤の有機物分解反応によって基材が分解されることができ、この場合、基材の安定性が低下し、基材の分解によって有害物質が発生する余地があった。
iO2非結晶性ゾルは、付着力が優秀で、前記TiO2非結晶性ゾルをバインダーとして利用して形成された光触媒層30の透明性を確保するために有利である。
率を示すことができるので、別の紫外線供給装置を要しないこともある。
本発明の他の具体例において、チタン前駆体にアルコール溶媒及び酸を加えることで脱水及び脱アルコール反応によってTiO2非結晶性ゾルを得る段階;前記TiO2非結晶性ゾルを基材上に塗布及び乾燥してバリアー層を形成する段階;及び前記TiO2非結晶性ゾルに可視光活性光触媒剤粒子を混合して形成された組成物を前記バリアー層上に塗布及び乾燥して光触媒層を形成する段階;を含む、光触媒機能性フィルムの製造方法を提供する。
として使われ、窒酸、塩酸などの強酸を使うことができる。
実施例1
イソプロピルアルコールを溶媒としてチタンテトライソプロポキシド10wt%の溶液を作る。これを30分間撹拌した後、濃い窒酸を少量加えて加水分解した。その後、30分間撹拌することで、脱水、脱アルコールさせて非結晶性TiO2ゾルを作った。
基材上にバリアー層を形成したことを除いて、前記実施例1と同様の方法で光触媒機能性フィルムを製造した。
蒸溜水を溶媒にしてチタンテトライソプロポキシド10wt%の水溶液を作った後、これを撹拌して均一な沈殿物を生成した。この後、十分な量の窒酸を酸触媒として添加し、縮合重合で透明なゾルを得た。これを80℃で8時間以上撹拌して不透明な結晶性TiO2ゾルを製造した。
実施例1及び比較例1-2の光触媒層に対してホルムアルデヒド除去性能を評価した。実施例1及び比較例1-2で製作された光触媒層を20Lの小型チャンバー(ADTEC社製品)内に設けた後、0.08ppmのホルムアルデヒド濃度を有する清浄空気を167cc/minの流量で持続的に流し、換気回数が0.5回/hrになるようにした。光源としては10Wの白色蛍光灯を用い、照度が1000luxになるように設定した。ホルムアルデヒドの除去率は、チャンバーに入る前の濃度と、チャンバーを通った後の濃度を測定して計算した後、下記表1に記載した。濃度はDNPH(2,4-dinitrophenylhydrazine)カートリッジを利用して10Lに対する量を濃縮し、高性能液体クロマトグラフィー(HPLC、Agilent社製品)で分析した。
10:基材
20:バリアー層
30:光触媒層
Claims (14)
- 基材層、バリアー層、及び光触媒層の積層構造であって、
前記バリアー層は非結晶性TiO2膜であり、
前記光触媒層は可視光活性光触媒剤粒子を含む非結晶性TiO 2 膜である、光触媒機能性フィルム。 - 前記非結晶性TiO2膜の気孔度は5%ないし50%であることを特徴とする、請求項1に記載の光触媒機能性フィルム。
- 前記非結晶性TiO2膜の比表面積が5m2/gないし500m2/gであることを特徴とする、請求項1に記載の光触媒機能性フィルム。
- 前記非結晶性TiO2膜はTiO2非結晶性ゾルの乾燥物であることを特徴とする、請求項1に記載の光触媒機能性フィルム。
- 前記可視光活性光触媒剤粒子は、空隙を含む可視光活性付与金属を担持した多孔性金属酸化物粒子であることを特徴とする、請求項1に記載の光触媒機能性フィルム。
- 前記多孔性金属酸化物粒子は、酸化チタン、酸化タングステン、酸化亜鉛、酸化ニオビオム及びこれらの組み合わせから選ばれた少なくとも一つを含むことを特徴とする、請求項5に記載の光触媒機能性フィルム。
- タングステン、クロム、バナジウム、モリブデナム、銅、鉄、コバルト、マンガン、ニッケル、白金、金、セリウム、カドミウム、亜鉛、マグネシウム、カルシウム、ストロンチウム、バリウム、ラジウム及びこれらの組み合わせから選ばれた少なくとも一つの金属を含む可視光活性付与金属、またはこれらの酸化物の形で前記可視光活性付与金属が多孔性金属酸化物粒子に担持されたことを特徴とする、請求項5に記載の光触媒機能性フィルム。
- 前記可視光活性光触媒剤粒子は、多孔性金属酸化物に対し、可視光活性付与金属と可視光活性付与金属酸化物の和の重量比99.9:0.1ないし99:1の重量比で含むことを特徴とする、請求項1に記載の光触媒機能性フィルム。
- 前記バリアー層の厚さは20nmないし500nmであることを特徴とする、請求項1に記載の光触媒機能性フィルム。
- 前記光触媒層の厚さは50nmないし500nmであることを特徴とする、請求項1に記載の光触媒機能性フィルム。
- 前記基材は室内インテリア内装材であることを特徴とする、請求項1に記載の光触媒機能性フィルム。
- チタン前駆体にアルコール溶媒及び酸を加えて脱水及び脱アルコール反応によってTiO2非結晶性ゾルを得る段階;
前記TiO2非結晶性ゾルを基材上に塗布及び乾燥してバリアー層を形成する段階;及び
前記TiO2非結晶性ゾルに可視光活性光触媒剤粒子を混合して形成された組成物を前記バリアー層上に塗布及び乾燥して光触媒層を形成する段階;を含む、光触媒機能性フィルムの製造方法。 - 前記アルコール溶媒は、イソプロピルアルコール、エタノール、メタノール、ブタノール及びこれらの組み合わせからなる群より選ばれた少なくとも一つであることを特徴とする、請求項12に記載の光触媒機能性フィルム製造方法。
- 前記組成物は、可視光活性光触媒剤粒子100重量部に対して前記TiO2非結晶性ゾルを20ないし100重量部含むことを特徴とする、請求項12に記載の光触媒機能性フィルムの製造方法。
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