CN106000423B - TiO2/MnS/Ga2O3Composite photocatalyst colloid preparation method - Google Patents
TiO2/MnS/Ga2O3Composite photocatalyst colloid preparation method Download PDFInfo
- Publication number
- CN106000423B CN106000423B CN201610385545.8A CN201610385545A CN106000423B CN 106000423 B CN106000423 B CN 106000423B CN 201610385545 A CN201610385545 A CN 201610385545A CN 106000423 B CN106000423 B CN 106000423B
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- CN
- China
- Prior art keywords
- tio
- mns
- colloid
- composite photocatalyst
- manganese
- Prior art date
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 85
- 239000000084 colloidal system Substances 0.000 title claims abstract description 38
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 22
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- QZQVBEXLDFYHSR-UHFFFAOYSA-N gallium(III) oxide Inorganic materials O=[Ga]O[Ga]=O QZQVBEXLDFYHSR-UHFFFAOYSA-N 0.000 claims abstract description 57
- 239000002131 composite material Substances 0.000 claims abstract description 37
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims abstract description 27
- 239000007787 solid Substances 0.000 claims abstract description 6
- 238000001035 drying Methods 0.000 claims abstract description 4
- 150000001875 compounds Chemical class 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 11
- 238000003756 stirring Methods 0.000 claims description 11
- 239000000908 ammonium hydroxide Substances 0.000 claims description 9
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 8
- 238000000502 dialysis Methods 0.000 claims description 7
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 150000003608 titanium Chemical class 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 5
- CHPZKNULDCNCBW-UHFFFAOYSA-N gallium nitrate Chemical compound [Ga+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O CHPZKNULDCNCBW-UHFFFAOYSA-N 0.000 claims description 4
- 150000002696 manganese Chemical class 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
- 229910021529 ammonia Inorganic materials 0.000 claims description 3
- UOGMEBQRZBEZQT-UHFFFAOYSA-L manganese(2+);diacetate Chemical compound [Mn+2].CC([O-])=O.CC([O-])=O UOGMEBQRZBEZQT-UHFFFAOYSA-L 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 238000004064 recycling Methods 0.000 claims description 3
- 229910021380 Manganese Chloride Inorganic materials 0.000 claims description 2
- GLFNIEUTAYBVOC-UHFFFAOYSA-L Manganese chloride Chemical compound Cl[Mn]Cl GLFNIEUTAYBVOC-UHFFFAOYSA-L 0.000 claims description 2
- KKSAZXGYGLKVSV-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO KKSAZXGYGLKVSV-UHFFFAOYSA-N 0.000 claims description 2
- 238000001914 filtration Methods 0.000 claims description 2
- 229940044658 gallium nitrate Drugs 0.000 claims description 2
- 229940071125 manganese acetate Drugs 0.000 claims description 2
- 239000011565 manganese chloride Substances 0.000 claims description 2
- 235000002867 manganese chloride Nutrition 0.000 claims description 2
- 229940099607 manganese chloride Drugs 0.000 claims description 2
- 229940099596 manganese sulfate Drugs 0.000 claims description 2
- 239000011702 manganese sulphate Substances 0.000 claims description 2
- 235000007079 manganese sulphate Nutrition 0.000 claims description 2
- MIVBAHRSNUNMPP-UHFFFAOYSA-N manganese(2+);dinitrate Chemical compound [Mn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MIVBAHRSNUNMPP-UHFFFAOYSA-N 0.000 claims description 2
- SQQMAOCOWKFBNP-UHFFFAOYSA-L manganese(II) sulfate Chemical compound [Mn+2].[O-]S([O-])(=O)=O SQQMAOCOWKFBNP-UHFFFAOYSA-L 0.000 claims description 2
- YUKQRDCYNOVPGJ-UHFFFAOYSA-N thioacetamide Chemical compound CC(N)=S YUKQRDCYNOVPGJ-UHFFFAOYSA-N 0.000 claims description 2
- DLFVBJFMPXGRIB-UHFFFAOYSA-N thioacetamide Natural products CC(N)=O DLFVBJFMPXGRIB-UHFFFAOYSA-N 0.000 claims description 2
- JMXKSZRRTHPKDL-UHFFFAOYSA-N titanium ethoxide Chemical compound [Ti+4].CC[O-].CC[O-].CC[O-].CC[O-] JMXKSZRRTHPKDL-UHFFFAOYSA-N 0.000 claims description 2
- 229910000349 titanium oxysulfate Inorganic materials 0.000 claims description 2
- 239000003292 glue Substances 0.000 claims 1
- 230000003647 oxidation Effects 0.000 abstract description 6
- 238000007254 oxidation reaction Methods 0.000 abstract description 6
- 238000006555 catalytic reaction Methods 0.000 abstract description 5
- 239000011248 coating agent Substances 0.000 description 20
- 238000000576 coating method Methods 0.000 description 20
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 18
- 239000003054 catalyst Substances 0.000 description 13
- 238000005507 spraying Methods 0.000 description 12
- 239000003795 chemical substances by application Substances 0.000 description 10
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 9
- 239000000243 solution Substances 0.000 description 9
- 239000000919 ceramic Substances 0.000 description 7
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 6
- 238000000034 method Methods 0.000 description 6
- 238000004140 cleaning Methods 0.000 description 5
- 230000001699 photocatalysis Effects 0.000 description 5
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 4
- 230000015556 catabolic process Effects 0.000 description 4
- 238000006731 degradation reaction Methods 0.000 description 4
- 235000019441 ethanol Nutrition 0.000 description 4
- 238000005286 illumination Methods 0.000 description 4
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
- 239000004033 plastic Substances 0.000 description 4
- 239000007921 spray Substances 0.000 description 4
- -1 SiO2 Chemical class 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 210000003195 fascia Anatomy 0.000 description 3
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- 239000010438 granite Substances 0.000 description 3
- 238000007146 photocatalysis Methods 0.000 description 3
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 3
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Substances [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 238000007761 roller coating Methods 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- 239000000377 silicon dioxide Substances 0.000 description 3
- CADICXFYUNYKGD-UHFFFAOYSA-N sulfanylidenemanganese Chemical compound [Mn]=S CADICXFYUNYKGD-UHFFFAOYSA-N 0.000 description 3
- 229910052717 sulfur Inorganic materials 0.000 description 3
- 230000010148 water-pollination Effects 0.000 description 3
- 239000011787 zinc oxide Substances 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 description 2
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical class O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 2
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 2
- 239000000853 adhesive Substances 0.000 description 2
- 230000001070 adhesive effect Effects 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- 230000000844 anti-bacterial effect Effects 0.000 description 2
- 239000004566 building material Substances 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- AJNVQOSZGJRYEI-UHFFFAOYSA-N digallium;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Ga+3].[Ga+3] AJNVQOSZGJRYEI-UHFFFAOYSA-N 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000011156 evaluation Methods 0.000 description 2
- 229910052733 gallium Inorganic materials 0.000 description 2
- 229910001195 gallium oxide Inorganic materials 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 229910052737 gold Inorganic materials 0.000 description 2
- 230000007062 hydrolysis Effects 0.000 description 2
- 238000006460 hydrolysis reaction Methods 0.000 description 2
- AMWRITDGCCNYAT-UHFFFAOYSA-L hydroxy(oxo)manganese;manganese Chemical compound [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 229910052500 inorganic mineral Inorganic materials 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 2
- 239000004922 lacquer Substances 0.000 description 2
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 description 2
- 229940040145 liniment Drugs 0.000 description 2
- 239000000865 liniment Substances 0.000 description 2
- 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 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- CEQFOVLGLXCDCX-WUKNDPDISA-N methyl red Chemical compound C1=CC(N(C)C)=CC=C1\N=N\C1=CC=CC=C1C(O)=O CEQFOVLGLXCDCX-WUKNDPDISA-N 0.000 description 2
- 229910052759 nickel Inorganic materials 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 239000005416 organic matter Substances 0.000 description 2
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- 229910052697 platinum Inorganic materials 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
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- 238000011160 research Methods 0.000 description 2
- 229910052706 scandium Inorganic materials 0.000 description 2
- SIXSYDAISGFNSX-UHFFFAOYSA-N scandium atom Chemical compound [Sc] SIXSYDAISGFNSX-UHFFFAOYSA-N 0.000 description 2
- 229910052709 silver Inorganic materials 0.000 description 2
- 229910052725 zinc Inorganic materials 0.000 description 2
- 239000011701 zinc Substances 0.000 description 2
- HIXDQWDOVZUNNA-UHFFFAOYSA-N 2-(3,4-dimethoxyphenyl)-5-hydroxy-7-methoxychromen-4-one Chemical compound C=1C(OC)=CC(O)=C(C(C=2)=O)C=1OC=2C1=CC=C(OC)C(OC)=C1 HIXDQWDOVZUNNA-UHFFFAOYSA-N 0.000 description 1
- 239000005995 Aluminium silicate Substances 0.000 description 1
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- 229910052684 Cerium Inorganic materials 0.000 description 1
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 239000005749 Copper compound Substances 0.000 description 1
- 239000005751 Copper oxide Substances 0.000 description 1
- 239000004606 Fillers/Extenders Substances 0.000 description 1
- PXGOKWXKJXAPGV-UHFFFAOYSA-N Fluorine Chemical compound FF PXGOKWXKJXAPGV-UHFFFAOYSA-N 0.000 description 1
- 239000005909 Kieselgur Substances 0.000 description 1
- 229910052779 Neodymium Inorganic materials 0.000 description 1
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- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Chemical compound [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 description 1
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- XBVKWSZUBPXCHZ-UHFFFAOYSA-N butan-1-ol;manganese Chemical compound [Mn].CCCCO XBVKWSZUBPXCHZ-UHFFFAOYSA-N 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 229910000019 calcium carbonate Inorganic materials 0.000 description 1
- 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 1
- 229910000420 cerium oxide Inorganic materials 0.000 description 1
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- 238000012790 confirmation Methods 0.000 description 1
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- 150000001880 copper compounds Chemical class 0.000 description 1
- 229910000431 copper oxide Inorganic materials 0.000 description 1
- 229910052593 corundum Inorganic materials 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- TYIXMATWDRGMPF-UHFFFAOYSA-N dibismuth;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Bi+3].[Bi+3] TYIXMATWDRGMPF-UHFFFAOYSA-N 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
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- RTZKZFJDLAIYFH-UHFFFAOYSA-N ether Substances CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 1
- 238000006266 etherification reaction Methods 0.000 description 1
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- PJXISJQVUVHSOJ-UHFFFAOYSA-N indium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[In+3].[In+3] PJXISJQVUVHSOJ-UHFFFAOYSA-N 0.000 description 1
- 125000001449 isopropyl group Chemical group [H]C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 1
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 description 1
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- QEFYFXOXNSNQGX-UHFFFAOYSA-N neodymium atom Chemical compound [Nd] QEFYFXOXNSNQGX-UHFFFAOYSA-N 0.000 description 1
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- 229910017604 nitric acid Inorganic materials 0.000 description 1
- QGLKJKCYBOYXKC-UHFFFAOYSA-N nonaoxidotritungsten Chemical compound O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1 QGLKJKCYBOYXKC-UHFFFAOYSA-N 0.000 description 1
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- 150000002927 oxygen compounds Chemical class 0.000 description 1
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- SNGREZUHAYWORS-UHFFFAOYSA-N perfluorooctanoic acid Chemical compound OC(=O)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)F SNGREZUHAYWORS-UHFFFAOYSA-N 0.000 description 1
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- 238000003980 solgel method Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
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- 229910052950 sphalerite Inorganic materials 0.000 description 1
- 230000001954 sterilising effect Effects 0.000 description 1
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- 229910052682 stishovite Inorganic materials 0.000 description 1
- 239000000454 talc Substances 0.000 description 1
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- 235000012222 talc Nutrition 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
- 239000011135 tin Substances 0.000 description 1
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 1
- 229910001887 tin oxide Inorganic materials 0.000 description 1
- QHGNHLZPVBIIPX-UHFFFAOYSA-N tin(II) oxide Inorganic materials [Sn]=O QHGNHLZPVBIIPX-UHFFFAOYSA-N 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
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- GPPXJZIENCGNKB-UHFFFAOYSA-N vanadium Chemical compound [V]#[V] GPPXJZIENCGNKB-UHFFFAOYSA-N 0.000 description 1
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- 229910001845 yogo sapphire Inorganic materials 0.000 description 1
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- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 description 1
- 229910052984 zinc sulfide Inorganic materials 0.000 description 1
- 229910001928 zirconium oxide Inorganic materials 0.000 description 1
Classifications
-
- 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
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Abstract
The invention discloses a kind of TiO2/MnS/Ga2O3Composite photocatalyst colloid preparation method, includes the following steps:1)Synthesize TiO2Colloidal sol 2)Synthesize Ga2O3Colloidal sol 3)Synthesize cotton-shaped MnS 4)TiO2/MnS/Ga2O3Composite photocatalyst colloid synthesizes:By step 1), step 2)Prepared TiO2Colloidal sol, Ga2O3Colloidal sol mixes, TiO2/MnS/Ga2O3TiO in solid after the drying of composite photocatalyst colloid290.0~97.0 wt% of content, MnS contents 2.9~8.0 wt%, Ga2O30.1~2.0 wt% of content;Sun light utilization efficiency of the present invention is high and catalysis oxidation ability is strong.
Description
Technical field
The invention belongs to catalysis material technical fields, and in particular to a kind of TiO2/MnS/Ga2O3Composite photocatalyst colloid
Preparation method.
Background technology
With the improvement of living standards, people increasingly pay attention to environmental problem, but the often means or medicine of environmental improvement
Object brings new pollution, such as chemosterilant or decontaminant again in itself.In recent years, at a kind of environment using photocatalysis principle
Reason is gradually popular with protection technique, and maximum advantage is not generate secondary pollution, directly by gas phase or liquid phase organic pollution
It resolves into environmentally friendly inorganic mineral and achievees the purpose that automatically cleaning, purification air and antibacterial.Wherein TiO2Photochemical catalyst because
Its excellent physicochemical property be used to prepare the coating with above-mentioned environment-friendly function in recent years.But due to pure TiO2Photo-quantum efficiency
It is low, therefore pure TiO2The use of light catalyzed coating is restricted.
In order to improve the activity of light catalyzed coating, from the angle of composition, the TiO of commercialization at present2Base optic catalytic coating can
It is roughly divided into three classes:1. with metal(Such as Au, Ag, Pt, Cu, Fe, Sn and Zn)It is or nonmetallic(C, N, S and P etc.)Doping;2. one
Kind or a variety of semiconductors(Such as ZnO, ZnS, SnO, Fe2O3、MnO、CeO2With CuO etc.)With TiO2It is compound;③TiO2With inertia oxygen
Compound(Such as SiO2、ZrO、Al2O3And diatomite and various clays etc.)It is compound.From literature search situation analysis, above-mentioned three kinds of structures
The photochemical catalyst of type is applied to prepare the light catalyzed coating with automatically cleaning, decomposing organic matter and anti-microbial property.And from system
Preparation Method angle, due to the limitation of coating characteristic, preparation method but only has a limited number of type:
First, photochemical catalyst is added to as filler in coating so that the coating has photocatalytic activity.This respect has
Representative patent includes the TiO that application number includes 201480027369.X2With copper compound composite coating,
201510630656.6 invention content adulterates TiO for Fe2, 201410781164.2 be TiO2Nanotube is scattered in inorganic coating
In, 201410104099.X as Cu-La adulterate TiO2It is scattered in coating, 201410228021.9 adulterate TiO for Fe-N2
It is scattered in coating, 201410123139.5 be single TiO2It is scattered in paint, 200510011793.8 adulterate TiO for N2。
Second is that the technology that photochemical catalyst is used directly as coating, the representative patent of this respect includes:
201410839055.1 it is by TiO2With inert diatomaceous earth it is compound, 201310169053.1 be by TiO2The direct roller coating of colloidal sol,
201110196966.3 it is by the TiO containing silver-copper-quaternary ammonium hydroxide2Mixture, 201110105280.9 are nanoparticles containing Au
Sub- TiO2Colloidal sol, 200710065676.9 are containing various metals(Silver, platinum, gold, palladium, scandium, vanadium, chromium, manganese, iron, cobalt, nickel, copper,
Zinc, scandium, yttrium, lanthanum, cerium, praseodymium, neodymium), it is nonmetallic(Nitrogen, carbon, sulphur, fluorine, boron)And oxide(Silica, aluminium oxide, tin oxide,
Iron oxide, tungsten oxide, zirconium oxide, zinc oxide, vanadium oxide, manganese oxide, oxidation tweezer, copper oxide, indium oxide, cerium oxide, bismuth oxide,
Lanthana, neodymia)TiO2Colloidal sol.
Third, photochemical catalyst solid, which is dispersed in adhesive, becomes coating, the representative patent of this respect includes:
201510425462.2 by TiO2It is dispersed in organic bond, additional inorganic mineral extenders(Calcium carbonate, kaolin, silica,
Talcum, quartz and barite), 201420827950.7 pass through Ca (OH)2Bond TiO2。
However the sun light utilization efficiency and catalysis oxidation ability of above-mentioned existing photochemical catalyst be not high.
Invention content
The technical problems to be solved by the invention are the shortcomings that overcoming the more than prior art:A kind of sunlight is provided to utilize
Rate is high and catalysis oxidation ability is strong is mainly used for photocatalytic self-cleaning, degradable organic pollutant and antibacterial and goes out virus
TiO2/MnS/Ga2O3Composite photocatalyst colloid preparation method.
The technical solution of the present invention is as follows:A kind of TiO2/MnS/Ga2O3Composite photocatalyst colloid preparation method, including
Following steps:
1)Synthesize TiO2Colloidal sol:Titanium salt is dissolved in absolute ethyl alcohol first, then by be configured to deionized water 1~
The salpeter solution of 5w% is heated to 10~90 DEG C, instills the above-mentioned absolute ethyl alcohol for having dissolved titanium salt under stiring, is persistently stirred after dripping off
It mixes 4~24 hours, obtains light blue transparent TiO2Colloid, the TiO2TiO in colloid2Content is controlled in 1.0~7.0wt%;
2)Synthesize Ga2O3Colloidal sol:Gallium nitrate is dissolved in the salpeter solution of 4~8wt% first, stir evenly and is heated to
10~50 DEG C, ammonium hydroxide is instilled under stiring, is persistently stirred 10~48 hours again after dripping off ammonium hydroxide, is obtained the Ga of pale yellow transparent2O3
Colloid, the Ga2O3Ga in colloid2O3Content is controlled in 0.1~2.0wt%;
3)Synthesize cotton-shaped MnS:Manganese salt is dissolved in the solution that a concentration of 1~8wt% is configured in deionized water first, so
TAA is instilled into above-mentioned solution afterwards, cotton-shaped MnS is obtained by filtration;
4)TiO2/MnS/Ga2O3Composite photocatalyst colloid synthesizes:By step 1), step 2)Prepared TiO2Colloidal sol,
Ga2O3Colloidal sol mixes, and persistently stirs 1~6 hour;Then mixture is obtained into TiO by recycling dialysis to pH=2~62/Ga2O3
Composite colloid;Again by the TiO2/Ga2O3Composite colloid and step 3)Cotton-shaped MnS mixing;Finally obtained solid content for 2~
The TiO of 4wt%2/MnS/Ga2O3Composite photocatalyst colloid, wherein, TiO2/MnS/Ga2O3After the drying of composite photocatalyst colloid
TiO in solid290.0~97.0 wt% of content, MnS contents 2.9~8.0 wt%, Ga2O30.1~2.0 wt% of content.
The titanium salt is one or more of titanium ethanolate, isopropyl titanate, butanol titanium and titanyl sulfate.
The manganese salt is one kind in manganese acetate, ethyl alcohol manganese, isopropanol manganese, butanol manganese, manganese nitrate, manganese chloride and manganese sulfate
It is or several.
The mass percentage concentration of ammonia is 20~28w% in the ammonium hydroxide.
The beneficial effects of the invention are as follows:The present invention is by TiO2、Ga2O3With MnS three it is compound form ternary photochemical catalyst,
The present invention is not only to propose completely new component combination, and its mechanism of action is different from the above-mentioned photochemical catalyst reported.
From functional perspective, single TiO had both been overcome2Photochemical catalyst cannot utilize sunlight middle-ultraviolet lamp(Compare visible light wave in sunlight
The section higher wave band of energy density)The shortcomings that, and improve the catalysis oxidation ability of composite photo-catalyst.That is, and TiO2
It compares, composite photo-catalyst of the invention will absorb more broadband sunlight(From ultraviolet to visible ray)Energy has simultaneously
Stronger redox ability.Ga2O3It is also a kind of semiconductor light-catalyst, although people are nothing like TiO to its research2、
ZnO and Fe2O3Etc. common photochemical catalyst, but one-component Ga2O3Photocatalysis performance be studied confirmation, such as the 14th is complete
State youth is catalyzed academic meeting paper《Out-phase knot (TiO2、Ga2O3) effect in photocatalysis》(2013),《It is catalyzed journal》
The paper delivered《Perfluoro caprylic acid in nano whiskers gallium oxide photocatalytic degradation pure water and waste water》(2013,34(8), 1551-
1559), Qingdao Technological University master thesis《Gallium oxide photocatalytic degradation repefral(DMP)And power
Learn research》(2013).Above-mentioned pure Ga2O3Photochemical catalyst result of study shows that although its oxidability is stronger, in sunlight
Under photocatalytic activity it is relatively low, main cause is pure Ga2O3It is only capable of absorbing the ultraviolet light for being shorter than 254nm.By Ga2O3As compound
One of component is the photochemical catalytic oxidation ability in order to improve compound, that is, improves coating decomposing pollutant, automatically cleaning and sterilizing
Performance.MnS is also semiconductor, and corresponding visible ray, but its oxidability is weaker, separately as photochemical catalyst effect and pays no attention to
Think.In previous paper and patent, also few trace in relation to its compound.But it absorbs the photoproduction current-carrying generated after visible ray
Son will transfer to TiO in the appropriate band structure of compound2Valence band or conduction band on and play a role.Colloid is made in compound
Form is the perfect condition of coating products, but prepares TiO2/MnS/Ga2O3The where the shoe pinches of composite colloid be containing Ti, Ms,
The predecessor dispergation speed of Ga and S and condition require differ greatly, by hydrolysis, hydro-thermal or solvent heat for usually preparing colloid etc. into
Gluing method is difficult to obtain desired compound, and preparation method provided by the invention solves the technical problem.The system of the present invention
Preparation Method is related to the combination of sol-gel method, the precipitation method and dialysis three.TiO2, MnS and Ga2O3Predecessor type and its
Hydrolysis rate difference is larger, if undergoing identical course under same environment as usually(Including temperature, pressure, time
With medium etc.), three must successively be formed, therefore final product is difficult to be formed the compound of uniform, high degree of mixing.The present invention uses
Substep plastic method, i.e., be respectively formed oxide first(TiO2And Ga2O3)Then colloidal sol prepares sulfide(MnS)Flocculent deposit,
Above-mentioned colloidal sol and precipitation are finally mixed, and is processed into product under given conditions.
Specific embodiment
The present invention is described in further details with specific embodiment below, but the present invention is not only limited in detail below in fact
Apply example.
Embodiment 1
First, 100ml deionized waters are measured and pours beaker into, then measured 2ml concentrated nitric acids and carefully, slowly prolong wall inflow water
In, it is stirred and heated to 45 DEG C.18ml isopropyl titanates are rapidly joined in 15ml absolute ethyl alcohols and stirred evenly in draught cupboard,
The ethanol solution of isopropyl titanate is slowly dropped under vigorous stirring in above-mentioned salpeter solution.Continue strongly after adding isopropyl titanate
Stirring 6 hours, obtained light blue transparent TiO2Colloid is spare.
Second, by 2.2g gallium nitrates(Purity 99%)It is dissolved in the aqueous solution of nitric acid of 100ml, 7w%, stirs evenly and adds
Heat is slowly dropped into ammonium hydroxide to 45 DEG C under being stirred strongly in draught cupboard(Containing ammonia 28%), drip off after ammonium hydroxide that persistently stirring 24 is small again
When, obtain pale yellow transparent Ga2O3Colloid is spare.
Third, 13g manganese acetates is taken to be dissolved in 100mL, 90 DEG C of deionized water, TAA is slowly added to after cooling while stirring
(Thioacetamide), until the molar ratio of Mn and S is 1:2.The manganese sulfide of generation largely sinks to as rufous flocculent deposit
Device bottom filters out red product and in order with ethyl alcohol, ether and purification water washing, obtains manganese sulfide floccule.
Fourth, by above-mentioned TiO2And Ga2O3Colloidal sol presses 50:1(Weight ratio)Ratio mixes, and persistently stirs 1 hour.Then will
Mixture obtains TiO by recycling dialyzer dialysis to pH=42/Ga2O3Composite colloid.
Fifth, by above-mentioned TiO2/Ga2O3Composite colloid and manganese sulfide floccule press 15:1(Weight ratio)Ratio is mixed and is added
Upper purified water 100ml, ultrasonic wave disperse after five minutes, strong stirring 24 hours.It can obtain TiO2/MnS/Ga2O3Complex light is urged
Change spray liniment.
Sixth, respectively by the pure TiO of 100ml2、Ga2O3And TiO2/MnS/Ga2O3Roller coating exists in two times for composite spraying agent
0.64M2(0.8Í0.8M)Without glaze polishing ceramic floor brick on(Polish that face), each time by 120 DEG C of bakings of Ceramic Tiles after roller coating
Dry 0.5hr, the three pieces of Ceramic Tiles that will obtain coating different coating in this way.
Seventh, the Ceramic Tiles of coated composite spraying agent are placed in 1M3It evaluates in case, it is molten to instill three drop formaldehyde using dropper
Liquid in as evaluation case in, be heated on 80 DEG C of nickel evaporating dish in advance, and rapidly close evaluate chamber door.Treat that concentration of formaldehyde records
Adsorption equilibrium is presented on instrument(Concentration is basically unchanged)Afterwards, ultraviolet lamp is opened(2 32W, 365nm ultraviolet lamps)And circulating fan, together
When start recording concentration of formaldehyde change with time situation.The result shows that after removing Natural Attenuation, concentration of formaldehyde is in 40min
0.04ppm is dropped to from 1.6ppm, degradation rate is more than 97%.Should statistics indicate that, coated with TiO2/MnS/Ga2O3Composite photocatalyst sprays
The building materials of paint have the function of fast decoupled pernicious gas.
Eighth, coated pure TiO2And Ga2O3Ceramic wafer also undergo same evaluation procedure respectively, the result is that:Pure TiO2
Ceramic wafer in 40min concentration of formaldehyde drop to 0.9ppm, degradation rate 40% from 1.5ppm.Pure Ga2O3Ceramic wafer in 40min
Concentration of formaldehyde drops to 1.4ppm, degradation rate 12% from 1.6ppm.That is, the sum of the two degradation rate only has 52%, far below equal conditions
Lower TiO2/MnS/Ga2O3The 97% of composite spraying agent.
Embodiment 2
One piece of the silvery white aluminium-plastic panel of 30cm × 30cm is taken, its surface is divided into equal two parts with blade(Every portion
Divide 450cm2).The TiO produced using embodiment 12/MnS/Ga2O3Composite spraying agent 5ml, is sprayed on above-mentioned aluminium-plastic panel in three times
A part therein, another part are covered as blank surface.By aluminium-plastic panel in 120 DEG C of drying after spraying each time
It is cool to room temperature finally to take out nature by 0.5hr.Commercially available pink is utilized on its surface(Based on methyl red)Watercolor stroke is no less than three
Road pink person's handwriting, per pass person's handwriting cross over two parts(Coat compound adhesive part and blank parts).Using a 8w,
All person's handwritings of 365nm ultra violet lamps, ultraviolet lamp is apart from plastic-aluminum plate surface 2cm.After 5min, coating composite spraying agent part plastic-aluminum
The pink person's handwriting of plate surface disappears(Methyl red is by photocatalytic degradation), and blank parts person's handwriting is still bright-coloured.The experiment shows
Coated with TiO2/MnS/Ga2O3The building materials of composite spraying agent (i.e. composite photocatalyst colloid) have fast decoupled organic pollution work(
Energy.
Embodiment 3
One piece of the canescence granite Side fascia of 80cm × 80cm is taken, its surface is divided into carbon marking pen equal
Two parts(Per part 800cm2).The TiO produced using embodiment 12/MnS/Ga2O3Composite spraying agent 8ml is sprayed on above-mentioned flower
A part for hilllock rock Side fascia, another part are covered as blank surface.More than 4hr is shone after spraying under sunlight.It utilizes
Contact angle instrument is measured in the granite Side fascia in ultraviolet lamp(Power 4W, dominant wavelength 365nm)Irradiation(Fluorescent tube and granite exterior wall
Plate distance 2cm)Front and rear contact angle situation of change.Contact-angle measurement major parameter is as follows:Medium is water, 0.5 μ l of droplet size,
Five measuring points are taken at random, finally calculate 5 points of average value.The result is that:Coated with TiO2/MnS/Ga2O3That face light of composite spraying agent
According to preceding 36 ° of average contact angle, illumination is averaged 2 ° after 0.5 hour.And blank surface illumination(Same version the other half, together
Etc. conditions illumination)It is front and rear at 36 °.This result shows that, which has fabulous photic hydrophily.Photic hydrophily is dropped with light
Solution organic matter ability is considered coating with two important elements of light self-cleaning property.
Embodiment 4
The TiO that will be obtained in embodiment 12/MnS/Ga2O3Composite spraying agent is packed into the dialysis bag of cutoff 20000,
Continuous dialysis 48hr, during which changes a deionized water per 12hr, obtains dialysis TiO again2/MnS/Ga2O3Composite spraying agent.By 3ml
The spray liniment disposable spray finishing tests photic hydrophily behind lacquer surface, naturally dry using the method that embodiment 3 provides.
The result shows that in lacquer surface sunlight(Towards southern metope, at 10 points in the morning starts)Illumination 20 minutes, 8 ° of water contact angle.
It the above is only the feature implementation example of the present invention, the scope of the present invention be not limited in any way.It is all to use together
The technical solution formed Deng exchange or equivalence replacement, all falls within rights protection scope of the present invention.
Claims (4)
1. a kind of TiO2/MnS/Ga2O3Composite photocatalyst colloid preparation method, it is characterised in that:Include the following steps:
1) TiO is synthesized2Colloidal sol:Titanium salt is dissolved in absolute ethyl alcohol first, it is dense then will to be configured to mass percent with deionized water
It spends and is heated to 10~90 DEG C for the salpeter solution of 1~5wt%, instill the above-mentioned absolute ethyl alcohol for having dissolved titanium salt under stiring, drip
It is persistently stirred after complete 4~24 hours, obtains light blue transparent TiO2Colloid, the TiO2TiO in colloid2Content is controlled in quality
Percent concentration is 1.0~7.0wt%;
2) Ga is synthesized2O3Colloidal sol:Gallium nitrate is dissolved in the salpeter solution that mass percent concentration is 4~8wt%, stirred first
It mixes uniformly and is heated to 10~50 DEG C, instill ammonium hydroxide under stiring, persistently stir 10~48 hours, obtain light again after dripping off ammonium hydroxide
The Ga of yellow transparent2O3Colloid, the Ga2O3Ga in colloid2O3Content control is 0.1~2.0wt% in mass percent concentration;
3) cotton-shaped MnS is synthesized:It is 1~8wt%'s manganese salt to be dissolved in first, mass percent concentration is configured in deionized water
Then solution instills thioacetamide into above-mentioned solution, cotton-shaped MnS is obtained by filtration;
4)TiO2/MnS/Ga2O3Composite photocatalyst colloid synthesizes:By the TiO prepared by step 1), step 2)2Colloidal sol, Ga2O3It is molten
Glue mixes, and persistently stirs 1~6 hour;Then mixture is obtained into TiO by recycling dialysis to pH=2~62/Ga2O3It is compound
Colloid;Again by the TiO2/Ga2O3Composite colloid and the cotton-shaped MnS of step 3) mixing;Finally obtained solid content is 2~4wt%
TiO2/MnS/Ga2O3Composite photocatalyst colloid, wherein, TiO2/MnS/Ga2O3Solid after the drying of composite photocatalyst colloid
Middle TiO2Content 90.0~97.0wt%, MnS content 2.9~8.0wt%, Ga2O30.1~2.0wt% of content.
2. TiO according to claim 12/MnS/Ga2O3Composite photocatalyst colloid preparation method, it is characterised in that:It is described
Titanium salt is one or more of titanium ethanolate, isopropyl titanate, butanol titanium and titanyl sulfate.
3. TiO according to claim 12/MnS/Ga2O3Composite photocatalyst colloid preparation method, it is characterised in that:It is described
Manganese salt is one or more of manganese acetate, manganese nitrate, manganese chloride and manganese sulfate.
4. TiO according to claim 12/MnS/Ga2O3Composite photocatalyst colloid preparation method, it is characterised in that:It is described
The mass percent concentration of ammonia is 20~28wt% in ammonium hydroxide.
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