CN106732612A - A kind of corronil nano wire/composite titania material and its preparation method and application - Google Patents
A kind of corronil nano wire/composite titania material and its preparation method and application Download PDFInfo
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- CN106732612A CN106732612A CN201611199923.XA CN201611199923A CN106732612A CN 106732612 A CN106732612 A CN 106732612A CN 201611199923 A CN201611199923 A CN 201611199923A CN 106732612 A CN106732612 A CN 106732612A
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- Prior art keywords
- corronil
- nano wire
- wire
- copper
- titania material
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 367
- 239000002070 nanowire Substances 0.000 title claims abstract description 217
- 239000000463 material Substances 0.000 title claims abstract description 111
- 239000002114 nanocomposite Substances 0.000 title claims abstract description 77
- 238000002360 preparation method Methods 0.000 title claims abstract description 38
- 239000004408 titanium dioxide Substances 0.000 claims abstract description 85
- 239000002131 composite material Substances 0.000 claims abstract description 37
- 229910000570 Cupronickel Inorganic materials 0.000 claims abstract description 35
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 32
- 239000000956 alloy Substances 0.000 claims abstract description 32
- YOCUPQPZWBBYIX-UHFFFAOYSA-N copper nickel Chemical compound [Ni].[Cu] YOCUPQPZWBBYIX-UHFFFAOYSA-N 0.000 claims abstract description 32
- 239000008187 granular material Substances 0.000 claims abstract description 19
- 238000011065 in-situ storage Methods 0.000 claims abstract description 6
- 238000000576 coating method Methods 0.000 claims description 104
- 239000011248 coating agent Substances 0.000 claims description 91
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 71
- 239000006185 dispersion Substances 0.000 claims description 40
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 27
- 239000010949 copper Substances 0.000 claims description 26
- 239000007788 liquid Substances 0.000 claims description 26
- 230000015556 catabolic process Effects 0.000 claims description 25
- 238000006731 degradation reaction Methods 0.000 claims description 25
- 229910052802 copper Inorganic materials 0.000 claims description 23
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 15
- 238000001291 vacuum drying Methods 0.000 claims description 15
- 239000002245 particle Substances 0.000 claims description 14
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 13
- 239000010936 titanium Substances 0.000 claims description 13
- 229910052719 titanium Inorganic materials 0.000 claims description 13
- 238000000137 annealing Methods 0.000 claims description 12
- VXUYXOFXAQZZMF-UHFFFAOYSA-N titanium(IV) isopropoxide Chemical group CC(C)O[Ti](OC(C)C)(OC(C)C)OC(C)C VXUYXOFXAQZZMF-UHFFFAOYSA-N 0.000 claims description 12
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 11
- 239000003054 catalyst Substances 0.000 claims description 11
- 238000005406 washing Methods 0.000 claims description 10
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 9
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 9
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 8
- 230000003197 catalytic effect Effects 0.000 claims description 8
- 239000003960 organic solvent Substances 0.000 claims description 6
- 239000002270 dispersing agent Substances 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 239000012298 atmosphere Substances 0.000 claims description 4
- 239000000725 suspension Substances 0.000 claims description 4
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- 230000004044 response Effects 0.000 claims description 2
- 230000002459 sustained effect Effects 0.000 claims description 2
- 229910000990 Ni alloy Inorganic materials 0.000 claims 1
- 239000002253 acid Substances 0.000 claims 1
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 claims 1
- 239000012855 volatile organic compound Substances 0.000 abstract description 8
- IKHGUXGNUITLKF-UHFFFAOYSA-N Acetaldehyde Chemical compound CC=O IKHGUXGNUITLKF-UHFFFAOYSA-N 0.000 abstract description 6
- 238000013033 photocatalytic degradation reaction Methods 0.000 abstract description 6
- 230000007062 hydrolysis Effects 0.000 abstract description 4
- 238000006460 hydrolysis reaction Methods 0.000 abstract description 4
- 238000007704 wet chemistry method Methods 0.000 abstract description 4
- 235000019441 ethanol Nutrition 0.000 description 51
- 239000007789 gas Substances 0.000 description 46
- 125000002485 formyl group Chemical class [H]C(*)=O 0.000 description 41
- 230000001699 photocatalysis Effects 0.000 description 33
- 239000000843 powder Substances 0.000 description 31
- 230000000052 comparative effect Effects 0.000 description 29
- 238000007146 photocatalysis Methods 0.000 description 27
- 238000006555 catalytic reaction Methods 0.000 description 21
- 230000000694 effects Effects 0.000 description 19
- 239000011521 glass Substances 0.000 description 16
- 238000005286 illumination Methods 0.000 description 16
- 238000000498 ball milling Methods 0.000 description 15
- 238000000034 method Methods 0.000 description 15
- 239000000523 sample Substances 0.000 description 15
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 14
- 238000001035 drying Methods 0.000 description 14
- 238000003756 stirring Methods 0.000 description 14
- 229910002482 Cu–Ni Inorganic materials 0.000 description 13
- 230000000593 degrading effect Effects 0.000 description 13
- 239000002103 nanocoating Substances 0.000 description 13
- 238000005457 optimization Methods 0.000 description 13
- 238000003908 quality control method Methods 0.000 description 13
- 239000004065 semiconductor Substances 0.000 description 13
- 125000005909 ethyl alcohol group Chemical group 0.000 description 11
- 239000002105 nanoparticle Substances 0.000 description 10
- 239000002243 precursor Substances 0.000 description 10
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 9
- 230000008859 change Effects 0.000 description 8
- 229910052751 metal Inorganic materials 0.000 description 8
- 239000002184 metal Substances 0.000 description 8
- 229910052724 xenon Inorganic materials 0.000 description 8
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 8
- 239000003638 chemical reducing agent Substances 0.000 description 7
- QNZRVYCYEMYQMD-UHFFFAOYSA-N copper;pentane-2,4-dione Chemical compound [Cu].CC(=O)CC(C)=O QNZRVYCYEMYQMD-UHFFFAOYSA-N 0.000 description 7
- 229910052759 nickel Inorganic materials 0.000 description 7
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 6
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 6
- 241000209094 Oryza Species 0.000 description 6
- 235000007164 Oryza sativa Nutrition 0.000 description 6
- 235000012149 noodles Nutrition 0.000 description 6
- 235000009566 rice Nutrition 0.000 description 6
- 239000003643 water by type Substances 0.000 description 6
- 239000012300 argon atmosphere Substances 0.000 description 5
- 230000002045 lasting effect Effects 0.000 description 5
- 239000002904 solvent Substances 0.000 description 5
- 239000000758 substrate Substances 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 239000010931 gold Substances 0.000 description 4
- 230000035484 reaction time Effects 0.000 description 4
- 241000790917 Dioxys <bee> Species 0.000 description 3
- 229910000792 Monel Inorganic materials 0.000 description 3
- 229910052786 argon Inorganic materials 0.000 description 3
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 description 3
- 125000002091 cationic group Chemical group 0.000 description 3
- 239000000356 contaminant Substances 0.000 description 3
- 239000011258 core-shell material Substances 0.000 description 3
- 230000005611 electricity Effects 0.000 description 3
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 3
- 229910052737 gold Inorganic materials 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 150000002815 nickel Chemical class 0.000 description 3
- 230000003287 optical effect Effects 0.000 description 3
- 150000003254 radicals Chemical class 0.000 description 3
- 239000004094 surface-active agent Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- FJLUATLTXUNBOT-UHFFFAOYSA-N 1-Hexadecylamine Chemical compound CCCCCCCCCCCCCCCCN FJLUATLTXUNBOT-UHFFFAOYSA-N 0.000 description 2
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 description 2
- 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 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 150000004945 aromatic hydrocarbons Chemical class 0.000 description 2
- 235000013339 cereals Nutrition 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000009833 condensation Methods 0.000 description 2
- 230000005494 condensation Effects 0.000 description 2
- 239000013068 control sample Substances 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 239000003344 environmental pollutant Substances 0.000 description 2
- 239000012467 final product Substances 0.000 description 2
- 230000003694 hair properties Effects 0.000 description 2
- 239000011261 inert gas Substances 0.000 description 2
- 229910001092 metal group alloy Inorganic materials 0.000 description 2
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 229910000510 noble metal Inorganic materials 0.000 description 2
- 150000002894 organic compounds Chemical class 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 239000011941 photocatalyst Substances 0.000 description 2
- 231100000719 pollutant Toxicity 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 2
- 241000208340 Araliaceae Species 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 206010013786 Dry skin Diseases 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- REYJJPSVUYRZGE-UHFFFAOYSA-N Octadecylamine Chemical compound CCCCCCCCCCCCCCCCCCN REYJJPSVUYRZGE-UHFFFAOYSA-N 0.000 description 1
- 235000005035 Panax pseudoginseng ssp. pseudoginseng Nutrition 0.000 description 1
- 235000003140 Panax quinquefolius Nutrition 0.000 description 1
- OUUQCZGPVNCOIJ-UHFFFAOYSA-M Superoxide Chemical compound [O-][O] OUUQCZGPVNCOIJ-UHFFFAOYSA-M 0.000 description 1
- GMMZXKSNKIUKOW-UHFFFAOYSA-N [O-2].[O-2].[Ti+4].C(C)O Chemical compound [O-2].[O-2].[Ti+4].C(C)O GMMZXKSNKIUKOW-UHFFFAOYSA-N 0.000 description 1
- 238000000862 absorption spectrum Methods 0.000 description 1
- IKHGUXGNUITLKF-XPULMUKRSA-N acetaldehyde Chemical compound [14CH]([14CH3])=O IKHGUXGNUITLKF-XPULMUKRSA-N 0.000 description 1
- MQRWBMAEBQOWAF-UHFFFAOYSA-N acetic acid;nickel Chemical compound [Ni].CC(O)=O.CC(O)=O MQRWBMAEBQOWAF-UHFFFAOYSA-N 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 150000003973 alkyl amines Chemical class 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 229910002056 binary alloy Inorganic materials 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 description 1
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 description 1
- 239000004567 concrete Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000009977 dual effect Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 235000008434 ginseng Nutrition 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 1
- -1 length is 1~20 μm Substances 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 239000002082 metal nanoparticle Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052961 molybdenite Inorganic materials 0.000 description 1
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 description 1
- 229910052982 molybdenum disulfide Inorganic materials 0.000 description 1
- 229940078494 nickel acetate Drugs 0.000 description 1
- AIYYMMQIMJOTBM-UHFFFAOYSA-L nickel(ii) acetate Chemical class [Ni+2].CC([O-])=O.CC([O-])=O AIYYMMQIMJOTBM-UHFFFAOYSA-L 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000010422 painting Methods 0.000 description 1
- HKJYVRJHDIPMQB-UHFFFAOYSA-N propan-1-olate;titanium(4+) Chemical compound CCCO[Ti](OCCC)(OCCC)OCCC HKJYVRJHDIPMQB-UHFFFAOYSA-N 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 229910021649 silver-doped titanium dioxide Inorganic materials 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000004528 spin coating Methods 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
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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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/74—Iron group metals
- B01J23/755—Nickel
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
- B01D53/86—Catalytic processes
- B01D53/8668—Removing organic compounds not provided for in B01D53/8603 - B01D53/8665
-
- 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
-
- 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
- B01J35/391—Physical properties of the active metal ingredient
- B01J35/393—Metal or metal oxide crystallite size
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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
- B01J35/40—Catalysts, in general, characterised by their form or physical properties characterised by dimensions, e.g. grain size
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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
- B01J35/50—Catalysts, in general, characterised by their form or physical properties characterised by their shape or configuration
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2257/00—Components to be removed
- B01D2257/70—Organic compounds not provided for in groups B01D2257/00 - B01D2257/602
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2257/00—Components to be removed
- B01D2257/70—Organic compounds not provided for in groups B01D2257/00 - B01D2257/602
- B01D2257/702—Hydrocarbons
- B01D2257/7027—Aromatic hydrocarbons
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2257/00—Components to be removed
- B01D2257/70—Organic compounds not provided for in groups B01D2257/00 - B01D2257/602
- B01D2257/708—Volatile organic compounds V.O.C.'s
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2259/00—Type of treatment
- B01D2259/80—Employing electric, magnetic, electromagnetic or wave energy, or particle radiation
- B01D2259/802—Visible light
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2259/00—Type of treatment
- B01D2259/80—Employing electric, magnetic, electromagnetic or wave energy, or particle radiation
- B01D2259/804—UV light
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- Chemical & Material Sciences (AREA)
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- Chemical Kinetics & Catalysis (AREA)
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- Environmental & Geological Engineering (AREA)
- Health & Medical Sciences (AREA)
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- Analytical Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
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Abstract
The present invention relates to a kind of corronil nano wire/composite titania material and its preparation method and application, the composite includes corronil nano wire and growth in situ in the titanium dioxide granule on the copper-nickel alloy nano-wire surface.The present invention uses wet chemistry method, in corronil nanowire surface hydrolysis growth titanium dioxide granule, so as to obtain corronil nano wire/composite titania material, and it is applied to photocatalytic degradation acetaldehyde under visible ray, reaches effectively degraded VOCs so as to the purpose of purify air.
Description
Technical field
Nano composite material and its preparation side the present invention relates to a kind of Novel Dual metal alloy semiconductor heterostructure
Method, belongs to the preparation field of catalysis material.
Background technology
Titanium dioxide (TiO2) due to excellent with physicochemical properties stabilization, chemically-resistant and photoetch, nontoxic, cheap etc.
Point, as a kind of preferable semi-conducting material, is widely used in solar cell, photocatalysis hydrogen production and photocatalytic degradation organic
The fields such as inorganic pollution.But TiO2Also there are some as a kind of exemplary wideband gap semiconductor material itself obvious not
Foot, its energy gap is excessive, and photoresponse scope is narrower, can only receive ultraviolet excitation;And TiO2Be stimulated the electron hole of generation
To easily compound, the reduction of photocatalysis efficiency is result in, it is there are many restrictions in actual applications.With opening for research
Exhibition, many people propose by adulterating or loading some elements or compound to improve TiO2Photocatalytic activity, can expand
Open up visible light-responded field (reference literature 1).
In recent years, many researchers attempt to construct energy by the way that titania nanoparticles are supported on different materials
Enough improve the heterojunction structure of photocatalysis efficiency, including Ag/TiO2, Cu/TiO2, CeO2/TiO2, Graphene/TiO2, MoS2/TiO2,
SnO2/TiO2Deng (reference literature 2-4).Wherein, metal/semiconductor heterostructure is partly led by improving photo-generated carrier in metal
Body interface efficiently separate so as to improve its light capture and photo-catalysis capability, additionally, metal due to its local surface etc. from
Daughter resonance effects, can not only improve the light absorbs of neighbouring semiconductor, and can be sensitized wide band gap semiconducter urges complex light
There is red shift in the absorption spectrum of agent, realize visible absorption.
B.Babu et al. has been synthesized with core by easy two steps wet chemistry method carried titanium dioxide on copper nano-wire
Copper metal nano wire/the composite titania material of shell structure, and have studied the composite material photocatalyst under ultraviolet light
To the photocatalytic degradation capability (reference literature 5) of liquid phase organic pollution.But, copper nano-wire/TiO2Material is because of its metal half
Schottky barrier is too low at conductor hetero-junctions, so as to be unfavorable for that the recombination rate for suppressing electron hole pair causes its light to a certain extent
Catalysis activity still has much room for improvement, and copper nano-wire/TiO2Material easily inactivates denaturation, greatly limit its practical application.This hair
Bright prepared corronil nano wire/composite titania material can effectively degrade the volatilization such as aldehydes gas under current system
Property organic compound, and Photocatalytic Degradation Property higher is respectively provided with ultraviolet light and visible ray.The composite has new
Newness and novelty, have broad application prospects in terms of removal haze precursor pollutant and indoor polluted gas.
Prior art literature:
Yi-Hsing Lin, Hsin-Ta Hsueh, the et al.Applied Catalysis B of document 1:Environmental
199(2016)1–10;
Changchao Jia, Ping Yang, the et al.ChemCatChem 2016,8,839-847 of document 2;
Weiwei Zhang, Hanlin Guo, the et al.Applied Surface Science 382 (2016) 128 of document 3-
134;
Yuxin Zhang, Ming Huang, the et al.J Mater Sci (2013) 48 of document 4:6728–6736;
Document 5 B.Babu, K.Mallikarjuna, et al.Materials Letters, 176 (2016) 265-269.
The content of the invention
Regarding to the issue above, it is an object of the invention to provide a kind of new binary metal alloy semiconductor heterojunction structure
Titanium dioxide base nano catalysis material and preparation method thereof, i.e., it is an object of the invention to provide a kind of corronil nanometer
Line/composite titania material and preparation method thereof, another object of the present invention is to provide a kind of corronil nano wire/bis-
Application of the titanium oxide composite material in purification of air.
On the one hand, the invention provides a kind of corronil nano wire/composite titania material (corronil nanometer
The catalysis material of line/titania nanoparticles semiconductor heterostructure), the composite includes corronil nano wire
And growth in situ is in the titanium dioxide granule on the copper-nickel alloy nano-wire surface.
The present invention is carried metal from corronil nano wire, and titanium dioxide granule is grown in its surface in situ, is obtained
A kind of high-performance optical catalyst with bimetallic semiconductor heterostructure.Wherein, corronil nano wire one-dimentional structure is in electricity
Sub- transmission aspect has unique advantage, quickly can be conducted electronics compared to for nano particle, accelerates photoproduction electricity
Son and the separation in hole, so that the recombination rate of photo-generate electron-hole is effectively inhibited, the photoproduction electricity separated under illumination condition
Son and hole can occur chemistry and send out that superoxide radical and hydroxyl should be generated with absorption in the oxygen and water etc. of material surface respectively
Free radical, the generation of more living radicals is so as to substantially increase the photocatalytic activity of composite.And corronil
The core shell structure of nano wire is made up of the copper core of internal layer and the nickel shell of outer layer, due to the nickel shell height stable homogeneous of its outer layer, copper
Nickel alloy nano wire shows significant stability within 65 DEG C of next months so that the composite material photocatalyst can be long-term
Keep high catalytic activity.
It is preferred that the weight ratio of the copper-nickel alloy nano-wire and titanium dioxide granule is (0.01~0.20):1, preferably
(0.01~0.05):1.
It is preferred that a diameter of 20~200nm of the copper-nickel alloy nano-wire, length is 1~20 μm, wherein copper and mickel
Mol ratio be (8~1):1, preferably 4:1.The core shell structure of the corronil nano wire uniqueness used in the present invention is by interior
The copper core of layer and the nickel shell composition of outer layer, the wherein mol ratio of copper and mickel is (8~1):1 (preferably 4:1) when, the nickel of its outer layer
Shell keeps height stable homogeneous substantially, just allows that the composite material photocatalyst keeps high catalytic activity for a long time.
It is preferred that the particle diameter of the titanium dioxide granule is 50~300nm, preferably 150~250nm.
On the other hand, present invention also offers a kind of preparation method of corronil nano wire/composite titania material,
Including:
Hanged to deionized water and organic titanium source, sustained response 0.5~24 hour is added in corronil nanowire dispersion
Turbid liquid;
By gained suspension through centrifuge washing, vacuum drying after, in inert atmosphere at 200~600 DEG C make annealing treatment 1~12
Hour, obtain the copper-nickel alloy nano-wire/composite titania material photochemical catalyst.
The present invention carries out isopropyl titanate hydrolysis generation titanium dioxide using wet chemistry method in corronil nanowire surface
Grain, obtains the copper-nickel alloy nano-wire/titanium dioxide that pattern coats corronil nano wire for titania nanoparticles
Composite.The present invention is prepared by normal temperature wet chemical method, and titania nanoparticles growth in situ is in corronil nanometer
Line surface forms the structure that titania nanoparticles coat corronil nano wire.In the composite that the present invention is provided,
Grain titania nanoparticles of uniform size are closely coated on around corronil nano wire, are a kind of new photocatalysis materials
Material, and by adjusting Cu-Ni nano wires and TiO in the heterojunction structure composite2Weight ratio, obtained different photocatalysis
Activity.
It is preferred that the dispersant of the copper-nickel alloy nano-wire dispersion liquid is organic solvent, preferably ethanol, methyl alcohol, different
At least one in propyl alcohol, ethylene glycol, toluene and acetone.
It is preferred that the organic titanium source is isopropyl titanate or butyl titanate.
It is preferred that the mol ratio of the copper-nickel alloy nano-wire and organic titanium source is (0.01~0.50):1, preferably (0.01
~0.20):1.
It is preferred that the inert gas is argon gas or nitrogen.
The third aspect, waves the invention provides a kind of corronil nano wire/composite titania material in catalytic degradation
Application in hair property organic compound (VOC).VOC be formaldehyde, acetaldehyde, benzene, toluene, aromatic hydrocarbon in its
Middle one kind.
Fourth aspect, the invention provides a kind of corronil nano wire/composite titania material coating.Its preparation side
Method:Above-mentioned corronil nano wire/composite titania material is disperseed by solvent, blade coating forms composite on substrate
Coating.The coating can effectively degrade gaseous contaminant under light illumination.
It is preferred that the solvent is ethanol.
Also, it is preferred that the copper-nickel alloy nano-wire/composite titania material is (1- with the ratio of the quality of solvent
10):(90-99).
It is preferred that the coated weight of the coating is every square metre of 10~20g.
The present invention uses wet chemistry method, in corronil nanowire surface hydrolysis growth titanium dioxide granule, so as to obtain
Corronil nano wire/composite titania material, and it is applied to photocatalytic degradation acetaldehyde under visible ray, reach effectively drop
Solution VOCs is so as to the purpose of purify air.Simultaneously by adjusting different Cu-Ni nano wires and TiO2Weight ratio, obtain visible
The optimal composite coating material of photocatalytic activity.
The preparation method of corronil nano wire/composite titania material that the present invention is provided has following features:
(1) present invention combines the corronil nano wire and traditional photocatalysis material of titanium dioxide of stable performance, into
Work(is prepared for the metal semiconductor heterogeneous structural nano composite with high catalytic performance, the presence energy of corronil nano wire
Enough photo-generate electron-holes that effectively suppresses can promote the composite system to generate more activity to being combined, under illumination condition
Free radical, so as to substantially increase the photocatalytic activity of traditional photocatalysis material of titanium dioxide;
(2) present invention process is simple, relatively low to experimental facilities requirement, and experimental raw is cheap and easy to get, the corronil nanometer for obtaining
Line/composite titania material had both maintained the crystal structure and composition of base semiconductor photochemical catalyst, while improve partly leading
The visible light photocatalysis active of body photochemical catalyst;
(3) the corronil nano wire/composite titania material aldehydes gas etc. that can effectively degrade prepared by the present invention are waved
Hair property organic compound, and Photocatalytic Degradation Property higher is respectively provided with ultraviolet light and visible ray.Material settling out is repeated
Utilize, had broad application prospects in terms of removal haze precursor pollutant and indoor polluted gas.
Brief description of the drawings
Fig. 1 is the SEM figures of the pure titinium dioxide sample of preparation in comparative example 1;
Fig. 2 is the TEM figures of the pure titinium dioxide sample of preparation in comparative example 1;
Fig. 3 is the SEM figures of the corronil nano wire/composite titania material of preparation in embodiment 1;
Fig. 4 is the TEM figures of the corronil nano wire/composite titania material of preparation in embodiment 1;
Fig. 5 is the SEM figures of the corronil nano wire/composite titania material of preparation in embodiment 2;
Fig. 6 is the TEM figures of the corronil nano wire/composite titania material of preparation in embodiment 2;
Fig. 7 is the SEM figures of the corronil nano wire/composite titania material of preparation in embodiment 3;
Fig. 8 is the TEM figures of the corronil nano wire/composite titania material of preparation in embodiment 3;
Fig. 9 is the SEM figures of the corronil nano wire/composite titania material of preparation in embodiment 4;
Figure 10 is the TEM figures of the corronil nano wire/composite titania material of preparation in embodiment 4;
Figure 11 is different corronil nano wire/TiO in comparative example 1-2 and embodiment 1-42The catalysis material system of part by weight
Standby composite coating distinguishes the degradation curve of aldehydes gas under visible light;
Figure 12 is different corronil nano wire/TiO in comparative example 1-2 and embodiment 1-42The catalysis material system of part by weight
Standby composite coating distinguishes the degradation curve of aldehydes gas under ultraviolet light;
Figure 13 is the SEM figures of the copper nano-wire/composite titania material of preparation in comparative example 5;
Figure 14 is the TEM figures of the copper nano-wire/composite titania material of preparation in comparative example 5;
Figure 15 is copper nano-wire/TiO prepared by comparative example 52Composite coating prepared by the catalysis material of part by weight is visible
The degradation curve of aldehydes gas under light;
Figure 16 is copper nano-wire/TiO prepared by comparative example 52Composite coating prepared by the catalysis material of part by weight is ultraviolet
The degradation curve of aldehydes gas under light.
Specific embodiment
The present invention is further illustrated below by way of following implementation methods, it should be appreciated that following implementation methods are merely to illustrate this
Invention, is not intended to limit the present invention.
The present invention is prepared by hydrolyzing generation titanium dioxide granule in the corronil nanowire surface with rock-steady structure
High-performance optical catalyst with bimetallic semiconductor heterostructure, preparation method is simple to operation, with corronil nanometer
Line is carried metal, has obtained Stability Analysis of Structures and the nano wire of the corronil with high visible light catalytic activity/titanium dioxide is multiple
Condensation material.
In the present invention, the copper-nickel alloy nano-wire/composite titania material (binary alloy nano line/titanium dioxide
Composite) include corronil nano wire and by ordinary-temp hydrolysis corronil nanowire surface growth in situ dioxy
Change titanium particle.Cu-Ni nano wires and TiO in the copper-nickel alloy nano-wire/composite titania material2Weight ratio can be
(0.01~0.20):1, preferably (0.01~0.05):1.Because the catalytic performance of composite and Cu-Ni nano wires and TiO2's
Weight ratio is relevant, when it is higher than 0.2 that Cu-Ni nano wires content is excessively mass ratio, because playing the two of main photocatalysis
Titanium oxide content is very few so the photocatalysis performance of composite is substantially reduced;When the very few i.e. mass ratio of Cu-Ni nano wire contents
During less than 0.01, because there is serious agglomeration phenomenon and cause the photocatalysis performance of composite equally to drop significantly in titanium dioxide granule
It is low, therefore Cu-Ni nano wires and TiO in the copper-nickel alloy nano-wire/composite titania material2Mass ratio can be (0.01
~0.20):1, preferably (0.01~0.05):1.The diameter of the copper-nickel alloy nano-wire can be 20~200nm, length be 1~
20μm.The particle diameter of the titanium dioxide granule can be 50~300nm, preferably 150~250nm.It is applicable to the growth present invention multiple
The unique core shell structure of the corronil nano wire of condensation material is made up of the copper core of internal layer and the nickel shell of outer layer, wherein copper and mickel
Mol ratio can be (8~1):1, preferably 4:1.
The present invention is with corronil nano wire as carried metal, isopropyl titanate or butyl titanate as organic titanium source, prepare
Novel semi-conductor heterojunction structure composite coating with high visible light catalytic activity, it is right under visible light to substantially increase
The degradation rate of aldehydes gas under current system, has widened the spectrum respective range of traditional titanium dioxide optical catalyst.The example below
Property explanation the present invention provide corronil nano wire/composite titania material preparation method.
The preparation of the dispersion in organic solvent of corronil nano wire.Corronil nano wire is dispersed in into dispersant (has
Machine solvent) in, the corronil nanowire dispersion of certain density stable homogeneous is obtained after ultrasonic disperse.Specifically, will
The corronil nano wire obtained by reducing acetylacetone copper method is first cleaned three times with isopropanol, then is cleaned with ethanol three times,
Last ultrasonic disperse obtains the corronil nanowire dispersion of stable homogeneous in dispersant.The copper-nickel alloy nano-wire
The dispersant of dispersion liquid can be organic solvent, preferably at least in ethanol, methyl alcohol, isopropanol, ethylene glycol, toluene and acetone
Kind.In addition, the preparation method of heretofore described corronil nano wire includes but are not limited to reduction acetylacetone copper method (ginseng
See patent 201410153158.2), as long as the copper-nickel alloy nano-wire can be prepared.Wherein reduce acetylacetone copper
Method includes:A) cationic surface active agent is dissolved in organic reducing agent;B) in the organic reducing agent obtained in step a)
Mantoquita (acetylacetone copper) is added as copper source, and adds noble metal nano particles as catalyst, under the first set point of temperature
Reaction;C) to adding nickel salt as nickel source in reacted reducing agent in step b), reacted under the second set point of temperature, gained is produced
Product are cleaned, dried, and obtain final product the copper-nickel alloy nano-wire.Described organic reducing agent can be chain alkyl amine.Described is organic
Reducing agent can be cetylamine or octadecylamine.The cationic surface active agent can be cetyl trimethylammonium bromide.It is described
Cationic surface active agent can be dissolved in organic reducing agent at 100-250 DEG C.The mantoquita can be acetylacetone copper.Institute
It can be nickel acetate to state nickel salt.The organic reducing agent, mantoquita, the mol ratio of nickel salt can be 330:(5~10):(2~15).It is described
The first set point of temperature can be 120-200 DEG C in step b), and the reaction time can be 2-15 hours.Noble metal nano in the step b)
Particle can be the Pt nano particles or Au nano particles synthesized in glycol system.The second set point of temperature can in the step c)
It it is 200-250 DEG C, the reaction time can be -10 hours 30 minutes.
The preparation of corronil nano wire/composite titania material.Add in corronil nano wire alcohol dispersion liquid
Enter appropriate amount of deionized water to hydrolyze titanium source, afterwards be stirred continuously it is lower by titanium source (such as isopropyl titanate, butyl titanate etc.) plus
Enter in corronil nanowire dispersion, fully persistently 0.5~24h of stirring, to complete reaction, obtains suspension.It is specific next
Say, the mol ratio of the copper-nickel alloy nano-wire and organic titanium source is (0.01~0.50):1, preferably (0.01~0.20):1.
By suspension washed for several times with organic solvent (for example, alcohol etc.) centrifugal filtration, afterwards vacuum drying obtain
Powder precursor, by the powder precursor in an inert atmosphere high annealing to complete the crystallization of anatase phase titanium dioxide, i.e.,
Obtain corronil nano wire/composite titania material.The rotating speed of centrifuge washing can be 1000~10000rpm.Vacuum drying
Temperature can be 50~80 DEG C, and drying time can be 2~12h.Atmosphere of inert gases can be argon gas or/and nitrogen.The annealing
Temperature can be 200~600 DEG C, and the time of annealing can be 1~12h.
As a detailed example, isopropyl titanate is added drop-wise in corronil nanowire dispersion, after stirring fully,
60 DEG C of dryings overnight in vacuum drying oven are put into after alcohol centrifuge washing 4 times, then corronil nanometer is obtained in argon gas high annealing
Line/composite titania material, wherein the amount of the isopropyl titanate for using and corronil nano wire is respectively 3~11ml and 0.02
~0.06g, mixing time one hour, annealing conditions are the 3h that anneals at 450 DEG C.
The present invention is combined using corronil nano wire/titanium dioxide that above-mentioned wet chemistry method has been obtained pattern stable homogeneous
Material.Understood referring to Fig. 1-8, the corronil nano wire/composite titania material pattern prepared by the above method is uniform
A diameter of 20~200nm of Stability Analysis of Structures, wherein corronil nano wire, length is 1~20 μm, the particle diameter of titanium dioxide granule
It is 50~300nm, preferably 150~250nm.
Corronil nano wire/composite titania material obtained above is passed through organic solvent (such as second by the present invention
Alcohol etc.) disperse, ball milling, blade coating can obtain corronil nano wire/composite titania material coating.It should be understood that above-mentioned blade coating
Mode be only example, can by other approach formed coating, such as spraying, spin coating etc..Following exemplary ground explanation cupro-nickel
The preparation method of alloy nano-wire/composite titania material coating.
Corronil nano wire/the composite titania material that will be obtained using the above method is with alcohol solvent (for example, second
Alcohol or water etc.) mixing and ball milling 1-48h formed solid content for 1-10% slurry, blade coating obtained on substrate corronil nanometer
Line/composite titania material coating, the coating can degrade gaseous contaminant under light illumination.The coating base plate is chosen as
Metal, ceramics or glass substrate.The copper-nickel alloy nano-wire/composite titania material coating coated weight can be every square metre
10~20g.
As a detailed example, gained corronil nano wire/composite titania material is dispersed in anhydrous second
In alcohol, by obtaining corronil nano wire/composite titania material alcohol dispersion liquid after ball milling, by the dispersion liquid in glass
Blade coating obtains corronil nano wire/titanium dioxide composite coating on substrate, and wherein corronil nano wire/titanium dioxide is combined
The consumption of material and ethanol is respectively 0.2g and 2g, and Ball-milling Time is 24h, and blade coating area is 5cm*10cm, and the composite coating is scraped
The quality of the corronil nano wire/composite titania material of painting is 0.01g.
Present invention also offers a kind of corronil nano wire/application of the composite titania material in purification of air,
The specifically application in degraded VOC (VOC), the VOC can be formaldehyde, second
Aldehyde, benzene, toluene, aromatic hydrocarbon etc..The copper-nickel alloy nano-wire/composite titania material coating is formed on a glass substrate
Coating, the coating can effectively degrade gaseous contaminant under light illumination.To above-mentioned gained composite coating respectively in visible ray and
Aldehydes gas test under photocatalytic degradation current system is carried out under ultraviolet light.Wherein the concentration of aldehydes gas can be 500ppm.Can
See that light illumination condition can be 4*65W fluorescent lamps, UV Light condition can be 500W xenon lamps.The copper-nickel prepared by the present invention is closed
Nanowires of gold/composite titania material can be 0.03%~60%, ultraviolet degradation to the Visible Light Induced Photocatalytic rate of aldehydes gas
Rate can be 0.03%~90%.Respectively it can be seen from Figure 11 and Figure 12, for using above method gained corronil nano wire/
The visible light photocatalysis active highest of composite titania material, wherein embodiment 2 (Cu-Ni wt%=3%), to acetaldehyde gas
The degradation rate of body reaches 56%, and the visible light photocatalysis active of embodiment 1 (Cu-Ni wt%=1%) is (right also above comparative example 1
Than sample coating of titanium dioxide), the photocatalytic activity of embodiment 3 (Cu-Ni wt%=5%) is then slightly below the (control sample of comparative example 1
Coating of titanium dioxide);While the active also highest of the ultraviolet light photocatalysis of embodiment 2 (Cu-Ni wt%=3%), to aldehydes gas
Degradation rate reach 88%, the ultraviolet light of embodiment 1 (Cu-Ni wt%=1%) and embodiment 3 (Cu-Ni wt%=5%) is urged
Change activity and be above comparative example 1 (control sample coating of titanium dioxide).
Embodiment is enumerated further below to describe the present invention in detail.It will similarly be understood that following examples are served only for this
Invention is further described, it is impossible to be interpreted as limiting the scope of the invention, those skilled in the art is according to this hair
Some nonessential modifications and adaptations that bright the above is made belong to protection scope of the present invention.Following examples are specific
Technological parameter etc. is also only that an example in OK range, i.e. those skilled in the art can be done properly by the explanation of this paper
In the range of select, and do not really want to be defined in the concrete numerical value of hereafter example.
The preparation embodiment of monel nano wire
0.5g cetyl trimethylammonium bromides are dissolved in 8g cetylamines first;It is subsequently adding 1.3g acetylacetone copper conducts
Copper source, and Pt nano particles are added as catalyst, to be reacted at 180 DEG C, the reaction time is 12 hours;Gone back to reacted again
Add 0.2g nickel acetates as nickel source in former agent, reacted at 210 DEG C, the reaction time is 2 hours, products obtained therefrom is cleaned, dried,
The copper-nickel alloy nano-wire is obtained final product, the wherein mol ratio of copper and mickel is 4:1.Following embodiments and comparative example, if without special theory
It is bright to use corronil nano wire manufactured in the present embodiment.
Embodiment 1
The corronil nano wire of 0.0272g is dispersed in ultrasonic disperse 30 minutes in 100ml ethanol, uniform and stable dispersion is obtained
Property good corronil nanowire dispersion, to 10ml deionized waters are added in the dispersion liquid, be added dropwise after lasting stirring
The isopropyl titanate of 10.06ml, continues to stir 1h, after being sufficiently stirred for, with the rotating speed alcohol centrifuge washing 4 times of 4000rpm, is being put into
In vacuum drying oven 60 DEG C vacuum drying 12h, then the powder precursor that will be obtained under an argon atmosphere 400 DEG C annealing 3h, that is, obtain
The weight ratio of corronil nano wire/composite titania material powder, wherein corronil nano wire is 1%.Referring to Fig. 3,
Fig. 4, its SEM figure and TEM figures for showing gained corronil nano wire/composite titania material powder, therefrom visible, gained
Corronil nano wire/composite titania material pattern stable homogeneous.Wherein a diameter of the 5 of corronil nano wire~
500nm, length is 1~20 μm, and the particle diameter of titanium dioxide granule is 1~200nm.
0.2g corronils nano wire/titanium dioxide powder is taken, adds 2g absolute ethyl alcohols, ball milling 24h to obtain corronil
Nano wire/titanium dioxide alcohol dispersion liquid, is scratched on the glass plate of 5cm*10cm, and natural drying obtains corronil and receives
Rice noodles/coating of titanium dioxide, the quality control of coating is 0.1g.
By degrading, aldehydes gas are tested, to be carried out to gained corronil nano wire/composite titania material coating
Catalysis activity under visible ray is characterized and performance optimization, and coating quality is 0.1g, and the initial concentration of aldehydes gas is 500ppm, can
See the fluorescent lamp that light illumination condition is 4*65W.The visible ray light of corronil nano wire/coating of titanium dioxide is urged in the present embodiment
Change performance and see that Figure 11, wherein S1 are sample described in embodiment 1, degradation rate is 46% (± 5%).
Embodiment 2
The corronil nano wire of 0.0412g is dispersed in ultrasonic disperse 30 minutes in 100ml ethanol, uniform and stable dispersion is obtained
Property good corronil nanowire dispersion, to 10ml deionized waters are added in the dispersion liquid, be added dropwise after lasting stirring
The isopropyl titanate of 4.978ml, continues to stir 1h, after being sufficiently stirred for, with the rotating speed alcohol centrifuge washing 4 times of 4000rpm, is being put into
In vacuum drying oven 60 DEG C vacuum drying 12h, then the powder precursor that will be obtained under an argon atmosphere 400 DEG C annealing 3h, that is, obtain
The weight ratio of corronil nano wire/composite titania material powder, wherein corronil nano wire is 3%.Referring to Fig. 5,
6, its SEM figure and TEM figures for showing gained corronil nano wire/composite titania material powder, therefrom visible, gained copper
Nickel alloy nano wire/composite titania material pattern stable homogeneous.Wherein a diameter of 5~500nm of corronil nano wire,
Length is 1~20 μm, and the particle diameter of titanium dioxide granule is 1~200nm.
0.2g corronils nano wire/titanium dioxide powder is taken, adds 2g absolute ethyl alcohols, ball milling 24h to obtain corronil
Nano wire/titanium dioxide alcohol dispersion liquid, is scratched on the glass plate of 5cm*10cm, and natural drying obtains corronil and receives
Rice noodles/coating of titanium dioxide, the quality control of coating is 0.1g.
By degrading, aldehydes gas are tested, to be carried out to gained corronil nano wire/composite titania material coating
Catalysis activity under visible ray is characterized and performance optimization, and coating quality is 0.1g, and the initial concentration of aldehydes gas is 500ppm, can
See the fluorescent lamp that light illumination condition is 4*65W.The visible ray light of corronil nano wire/coating of titanium dioxide is urged in the present embodiment
Change performance and see that Figure 11, wherein S2 are sample described in embodiment 2, degradation rate is 60% (± 5%).
Embodiment 3
The corronil nano wire of 0.0516g is dispersed in ultrasonic disperse 30 minutes in 100ml ethanol, uniform and stable dispersion is obtained
Property good corronil nanowire dispersion, to 10ml deionized waters are added in the dispersion liquid, be added dropwise after lasting stirring
The isopropyl titanate of 3.66ml, continues to stir 1h, after being sufficiently stirred for, with the rotating speed alcohol centrifuge washing 4 times of 4000rpm, is being put into
In vacuum drying oven 60 DEG C vacuum drying 12h, then the powder precursor that will be obtained under an argon atmosphere 400 DEG C annealing 3h, that is, obtain
The weight ratio of corronil nano wire/composite titania material powder, wherein corronil nano wire is 5%.Referring to Fig. 7,
8, its SEM figure and TEM figures for showing gained corronil nano wire/composite titania material powder, therefrom visible, gained copper
Nickel alloy nano wire/composite titania material pattern stable homogeneous.Wherein a diameter of 5~500nm of corronil nano wire,
Length is 1~20 μm, and the particle diameter of titanium dioxide granule is 1~200nm.
0.2g corronils nano wire/titanium dioxide powder is taken, adds 2g absolute ethyl alcohols, ball milling 24h to obtain corronil
Nano wire/titanium dioxide alcohol dispersion liquid, is scratched on the glass plate of 5cm*10cm, and natural drying obtains corronil and receives
Rice noodles/coating of titanium dioxide, the quality control of coating is 0.1g.
By degrading, aldehydes gas are tested, to be carried out to gained corronil nano wire/composite titania material coating
Catalysis activity under visible ray is characterized and performance optimization, and coating quality is 0.1g, and the initial concentration of aldehydes gas is 500ppm, can
See the fluorescent lamp that light illumination condition is 4*65W.The visible ray light of corronil nano wire/coating of titanium dioxide is urged in the present embodiment
Change performance and see that Figure 11, wherein S3 are sample described in embodiment 3, degradation rate is 18% (± 5%).
Embodiment 4
The corronil nano wire of 0.169g is dispersed in ultrasonic disperse 30 minutes in 100ml ethanol, uniform and stable dispersion is obtained
Property good corronil nanowire dispersion, to 10ml deionized waters are added in the dispersion liquid, 3.0ml is added dropwise after lasting stirring
Isopropyl titanate, continue to stir 1h, after being sufficiently stirred for, with the rotating speed alcohol centrifuge washing 4 times of 4000rpm, dried vacuum is being put into
In case 60 DEG C vacuum drying 12h, then the powder precursor that will be obtained under an argon atmosphere 400 DEG C annealing 3h, that is, obtain cupro-nickel conjunction
The weight ratio of nanowires of gold/composite titania material powder, wherein corronil nano wire is 20%.Referring to Fig. 9,10, its
The SEM figures and TEM figures of gained corronil nano wire/composite titania material powder are shown, therefrom visible, gained cupro-nickel is closed
Nanowires of gold/composite titania material pattern stable homogeneous.Wherein a diameter of 5~500nm of corronil nano wire, length
It it is 1~20 μm, the particle diameter of titanium dioxide granule is 1~200nm.
0.2g corronils nano wire/titanium dioxide powder is taken, adds 2g absolute ethyl alcohols, ball milling 24h to obtain corronil
Nano wire/titanium dioxide alcohol dispersion liquid, is scratched on the glass plate of 5cm*10cm, and natural drying obtains corronil and receives
Rice noodles/coating of titanium dioxide, the quality control of coating is 0.1g.
By degrading, aldehydes gas are tested, to be carried out to gained corronil nano wire/composite titania material coating
Catalysis activity under visible ray is characterized and performance optimization, and coating quality is 0.1g, and the initial concentration of aldehydes gas is 500ppm, can
See the fluorescent lamp that light illumination condition is 4*65W.The visible ray light of corronil nano wire/coating of titanium dioxide is urged in the present embodiment
Change performance and see that Figure 11, wherein S4 are sample described in embodiment 4, degradation rate is 7% (± 5%).
Embodiment 5
Corronil nano wire/the titanium dioxide powder of the preparation of 0.2g embodiments 1 is taken, adds 2g absolute ethyl alcohols, ball milling 24h to obtain
To corronil nano wire/titanium dioxide alcohol dispersion liquid, scratched on the glass plate of 5cm*10cm, natural drying is obtained
Corronil nano wire/coating of titanium dioxide, the quality control of coating is 0.1g.
By degrading, aldehydes gas are tested, to be carried out to gained corronil nano wire/composite titania material coating
Catalysis activity under ultraviolet light is characterized and performance optimization, and coating quality is 0.1g, and the initial concentration of aldehydes gas is 500ppm, purple
Outer smooth illumination condition is the xenon lamp of 500W.The ultraviolet light photocatalysis of corronil nano wire/coating of titanium dioxide in the present embodiment
Performance is shown in that Figure 12, wherein S1 are sample described in embodiment 1, and degradation rate is 80% (± 5%).
Embodiment 6
Take 0.2g embodiments 2 and prepare corronil nano wire/titanium dioxide powder, add 2g absolute ethyl alcohols, ball milling 24h to obtain
Corronil nano wire/titanium dioxide alcohol dispersion liquid, is scratched on the glass plate of 5cm*10cm, and natural drying obtains copper
Nickel alloy nano wire/coating of titanium dioxide, the quality control of coating is 0.1g.
By degrading, aldehydes gas are tested, to be carried out to gained corronil nano wire/composite titania material coating
Catalysis activity under ultraviolet light is characterized and performance optimization, and coating quality is 0.1g, and the initial concentration of aldehydes gas is 500ppm, purple
Outer smooth illumination condition is the xenon lamp of 500W.The ultraviolet light photocatalysis of corronil nano wire/coating of titanium dioxide in the present embodiment
Performance is shown in that Figure 12, wherein S2 are sample described in embodiment 2, and degradation rate is 89% (± 5%).
Embodiment 7
Take 0.2g embodiments 3 and prepare corronil nano wire/titanium dioxide powder, add 2g absolute ethyl alcohols, ball milling 24h to obtain
Corronil nano wire/titanium dioxide alcohol dispersion liquid, is scratched on the glass plate of 5cm*10cm, and natural drying obtains copper
Nickel alloy nano wire/coating of titanium dioxide, the quality control of coating is 0.1g.
By degrading, aldehydes gas are tested, to be carried out to gained corronil nano wire/composite titania material coating
Catalysis activity under ultraviolet light is characterized and performance optimization, and coating quality is 0.1g, and the initial concentration of aldehydes gas is 500ppm, purple
Outer smooth illumination condition is the xenon lamp of 500W.The ultraviolet light photocatalysis of corronil nano wire/coating of titanium dioxide in the present embodiment
Performance is shown in that Figure 12, wherein S3 are sample described in embodiment 3, and degradation rate is 68% (± 5%).
Embodiment 8
Take 0.2g embodiments 4 and prepare corronil nano wire/titanium dioxide powder, add 2g absolute ethyl alcohols, ball milling 24h to obtain
Corronil nano wire/titanium dioxide alcohol dispersion liquid, is scratched on the glass plate of 5cm*10cm, and natural drying obtains copper
Nickel alloy nano wire/coating of titanium dioxide, the quality control of coating is 0.1g.
By degrading, aldehydes gas are tested, to be carried out to gained corronil nano wire/composite titania material coating
Catalysis activity under ultraviolet light is characterized and performance optimization, and coating quality is 0.1g, and the initial concentration of aldehydes gas is 500ppm, purple
Outer smooth illumination condition is the xenon lamp of 500W.The ultraviolet light photocatalysis of corronil nano wire/coating of titanium dioxide in the present embodiment
Performance is shown in that Figure 12, wherein S4 are sample described in embodiment 4, and degradation rate is 10% (± 5%).
Comparative example 1 (is free of corronil nano wire)
To 10ml deionized waters are added in 100ml ethanol, it is sufficiently stirred for, the isopropyl titanate of 5.00ml is then added dropwise while stirring,
Continue to stir 1h, after being sufficiently stirred for, with the rotating speed alcohol centrifuge washing 4 times of 4000rpm, 60 DEG C of vacuum in vacuum drying oven is put into
Dry 12h, then the powder precursor that will be obtained is annealed in the Muffle furnace 3h at 400 DEG C, that is, titanium dioxide powder is obtained, referring to figure
1st, 2, its SEM figure for showing gained titanic oxide material powder, therefrom visible, gained titanic oxide material pattern stable homogeneous,
Even particle size, the particle diameter of titanium dioxide granule is 1~200nm.
0.2g pure titinium dioxide powders are taken, adds 2g absolute ethyl alcohols, ball milling 24h to obtain titanium dioxide alcohol dispersion liquid, will
On the glass plate of 5cm*10cm, natural drying obtains coating of titanium dioxide to its blade coating, and the quality control of coating is 0.1g.
By degrade aldehydes gas test, come gained coating of titanium dioxide is carried out the catalysis activity under visible ray characterize and
Performance optimizes, and coating quality is 0.1g, and the initial concentration of aldehydes gas is 500ppm, it is seen that light illumination condition is glimmering for 4*65W's
Light lamp.The visible light photocatalysis performance of coating of titanium dioxide is shown in that Figure 11 and Figure 15, wherein S5 are described in comparative example 1 in this comparative example
Sample, degradation rate is 37% (± 5%).
Comparative example 2 (is free of titanium dioxide)
By the preparation embodiment of above-mentioned monel nano wire by reducing the corronil nano wire that acetylacetone copper method is obtained
First cleaned with isopropanol three times, then cleaned with ethanol three times, finally take 0.2g ultrasonic disperses in ethanol, obtain stable homogeneous
Corronil nano wire alcohol dispersion liquid.Scratched on the glass plate of 5cm*10cm, natural drying obtains corronil and receives
Rice noodles coating, the quality control of coating is 0.1g.
By degrading, aldehydes gas are tested, to carry out the catalysis activity under visible ray to gained corronil nano wire coating
Characterize and performance optimization, coating quality is 0.1g, and the initial concentration of aldehydes gas is 500ppm, it is seen that light illumination condition is 4*
The fluorescent lamp of 65W.The visible light photocatalysis performance of corronil nano wire coating is shown in Figure 11 and Figure 15, wherein S6 in this comparative example
The sample described in comparative example 2, degradation rate is 3% (± 5%).
Comparative example 3 (is free of corronil nano wire)
The pure titinium dioxide powder of the preparation of 0.2g comparative examples 1 is taken, adds 2g absolute ethyl alcohols, ball milling 24h to obtain titanium dioxide ethanol
Dispersion liquid, is scratched on the glass plate of 5cm*10cm, and natural drying obtains coating of titanium dioxide, and the quality control of coating is
0.1g。
By degrading, aldehydes gas are tested, to carry out the catalysis activity table under ultraviolet light respectively to gained coating of titanium dioxide
Levy and performance optimization, coating quality is 0.1g, and the initial concentration of aldehydes gas is 500ppm, and UV Light condition is 500W's
Xenon lamp.The ultraviolet light photocatalysis performance of coating of titanium dioxide is shown in that Figure 12 and Figure 16, wherein S5 are described in comparative example 1 in this comparative example
Sample, degradation rate is 43% (± 5%).
Comparative example 4 (is free of titanium dioxide)
Take the corronil nano wire ultrasonic disperse of preparation embodiment preparation of the above-mentioned monel nano wires of 0.2g in ethanol,
Obtain the corronil nano wire alcohol dispersion liquid of stable homogeneous.Scratched on the glass plate of 5cm*10cm, spontaneously dried
Corronil nano wire coating is obtained, the quality control of coating is 0.1g.
By degrading, aldehydes gas are tested, to carry out the catalysis activity under ultraviolet light to gained corronil nano wire coating
Characterize and performance optimization, coating quality is 0.1g, and the initial concentration of aldehydes gas is 500ppm, and UV Light condition is 500W
Xenon lamp.The ultraviolet light photocatalysis performance of corronil nano wire coating is shown in that Figure 12 and Figure 16, wherein S6 are right in this comparative example
Sample described in ratio 4, degradation rate is 3% (± 5%).
Comparative example 5
The copper nano-wire of 0.0272g is dispersed in ultrasonic disperse 30 minutes in 100ml ethanol, uniform and stable favorable dispersibility is obtained
Corronil nanowire dispersion, to 10ml deionized waters are added in the dispersion liquid, the different of 10.06ml is added dropwise after lasting stirring
Titanium propanolate, continues to stir 1h, after being sufficiently stirred for, with the rotating speed alcohol centrifuge washing 4 times of 4000rpm, in vacuum drying oven is put into
60 DEG C vacuum drying 12h, then the powder precursor that will be obtained under an argon atmosphere 400 DEG C annealing 3h, that is, obtain corronil and receive
The weight ratio of rice noodles/composite titania material powder, wherein corronil nano wire is 1%.Referring to Figure 13, Figure 14, it shows
Go out the SEM figures and TEM figures of gained copper nano-wire/composite titania material powder, therefrom visible, gained copper nano-wire/dioxy
Change titanium composite material pattern stable homogeneous.Wherein a diameter of 5~500nm of copper nano-wire, length is 1~20 μm, titanium dioxide
The particle diameter of particle is 1~200nm.
0.2g copper nano-wires/titanium dioxide powder is taken, adds 2g absolute ethyl alcohols, ball milling 24h to obtain copper nano-wire/dioxy
Change titanium alcohol dispersion liquid, scratched on the glass plate of 5cm*10cm, natural drying obtains copper nano-wire/titanium dioxide and applies
Layer, the quality control of coating is 0.1g.
By degrading, aldehydes gas are tested, to carry out visible ray to gained copper nano-wire/composite titania material coating
Under catalysis activity characterize and performance optimization, coating quality is 0.1g, and the initial concentration of aldehydes gas is 500ppm, it is seen that light light
It is the fluorescent lamp of 4*65W according to condition.The visible light photocatalysis performance of copper nano-wire/coating of titanium dioxide is shown in figure in this comparative example
15, wherein Cu/TiO2Be comparative example 5 prepare copper nano-wire/composite titania material coating, its degradation rate be 28% (±
5%).
By degrading, aldehydes gas are tested, to carry out ultraviolet light to gained copper nano-wire/composite titania material coating
Under catalysis activity characterize and performance optimization, coating quality is 0.1g, and the initial concentration of aldehydes gas is 500ppm, ultraviolet light light
It is the xenon lamp of 500W according to condition.The ultraviolet light photocatalysis performance of corronil nano wire coating is shown in Figure 16 in this comparative example, wherein
Cu/TiO2It is copper nano-wire/composite titania material coating prepared by comparative example 5, its degradation rate is 62% (± 5%).
By prepared corronil nano wire/composite titania material, using online photocatalytic system and meteorological color
Spectrometer is studied its photocatalysis performance, and its test result is referring to table 1:
Table 1:Degradation rate tables of data of the corronil nano wire/composite titania material to mobile phase aldehydes gas
Industrial applicability:
What the present invention was provided prepares corronil nano wire/composite titania material method process is simple, will to experimental facilities
Ask relatively low, experimental raw is cheap and easy to get, the corronil nano wire/composite titania material for obtaining both had maintained matrix and partly led
The crystal structure and composition of body photochemical catalyst, while improve the visible light photocatalysis active of semiconductor light-catalyst;And this hair
Bright prepared corronil nano wire/composite titania material coating can effectively degrade aldehydes gas etc. under current system
VOC, and Photocatalytic Degradation Property higher is respectively provided with ultraviolet light and visible ray.Material settling out can be again
It is multiple to utilize, had broad application prospects in terms of removal haze precursor pollutant and indoor polluted gas.
Claims (10)
1. a kind of corronil nano wire/composite titania material, it is characterised in that the composite includes corronil
Nano wire and growth in situ are in the titanium dioxide granule on the copper-nickel alloy nano-wire surface.
2. corronil nano wire/composite titania material according to claim 1, it is characterised in that the copper-nickel
The mass ratio of alloy nano-wire and titanium dioxide granule is(0.01~0.20):1, preferably(0.01~0.05):1.
3. corronil nano wire/composite titania material according to claim 1 and 2, it is characterised in that the copper
A diameter of 20~200 nm of nickel alloy nano wire, length is 1~20 micron, and the mol ratio of wherein copper and mickel is(8~1):1,
Preferably 4:1.
4. the corronil nano wire/composite titania material according to any one of claim 1-3, its feature exists
In the particle diameter of the titanium dioxide granule is 50~300 nm, preferably 150~250 nm.
5. a kind of preparation method of corronil nano wire/composite titania material as any one of claim 1-4,
It is characterised in that it includes:
Hanged to deionized water and organic titanium source, sustained response 0.5~24 hour is added in corronil nanowire dispersion
Turbid liquid;
By gained suspension through centrifuge washing, vacuum drying after, in inert atmosphere at 200~600 DEG C annealing 1~
12 hours, obtain the copper-nickel alloy nano-wire/composite titania material photochemical catalyst.
6. preparation method according to claim 5, it is characterised in that the dispersant of the copper-nickel alloy nano-wire dispersion liquid
It is organic solvent, the preferably at least one in ethanol, methyl alcohol, isopropanol, ethylene glycol, toluene and acetone.
7. the preparation method according to claim 5 or 6, it is characterised in that the organic titanium source is isopropyl titanate or metatitanic acid
Four butyl esters.
8. the preparation method according to any one of claim 5-7, it is characterised in that the copper-nickel alloy nano-wire and have
The mol ratio of machine titanium source is(0.01~0.50):1, preferably(0.01~0.20):1.
9. a kind of corronil nano wire/composite titania material as any one of claim 1-4 is in catalytic degradation
Application in VOC.
10. a kind of coating including corronil nano wire/composite titania material any one of claim 1-4.
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CN109876843A (en) * | 2019-03-08 | 2019-06-14 | 北京化工大学 | Copper alloy modified titanic oxide/carbonitride heterojunction photocatalyst and preparation method |
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
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CN109499585A (en) * | 2018-12-06 | 2019-03-22 | 中国科学院上海硅酸盐研究所 | A kind of tantalum disulfide/composite titania material and its preparation method and application |
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CN109876843A (en) * | 2019-03-08 | 2019-06-14 | 北京化工大学 | Copper alloy modified titanic oxide/carbonitride heterojunction photocatalyst and preparation method |
CN111482617A (en) * | 2020-01-30 | 2020-08-04 | 浙江大学 | Preparation method of silver nanowire surface in-situ growth metal oxide core point composite material |
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