CN108906129A - It is a kind of based on composite electroless-plating fiber base nickel-loaded/optically catalytic TiO 2 degradable material preparation method - Google Patents
It is a kind of based on composite electroless-plating fiber base nickel-loaded/optically catalytic TiO 2 degradable material preparation method Download PDFInfo
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- CN108906129A CN108906129A CN201810654170.XA CN201810654170A CN108906129A CN 108906129 A CN108906129 A CN 108906129A CN 201810654170 A CN201810654170 A CN 201810654170A CN 108906129 A CN108906129 A CN 108906129A
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- fabric
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- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 48
- 239000002131 composite material Substances 0.000 title claims abstract description 47
- 238000007772 electroless plating Methods 0.000 title claims abstract description 22
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 239000000835 fiber Substances 0.000 title claims abstract description 17
- 239000000463 material Substances 0.000 title claims abstract description 13
- 229910052759 nickel Inorganic materials 0.000 title claims abstract description 13
- 229910010413 TiO 2 Inorganic materials 0.000 title claims abstract description 7
- 230000003197 catalytic effect Effects 0.000 title claims abstract description 7
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 74
- 239000004744 fabric Substances 0.000 claims abstract description 67
- 239000004408 titanium dioxide Substances 0.000 claims abstract description 32
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 claims abstract description 19
- 229920000767 polyaniline Polymers 0.000 claims abstract description 12
- 229910021543 Nickel dioxide Inorganic materials 0.000 claims abstract description 11
- 229910052763 palladium Inorganic materials 0.000 claims abstract description 9
- 239000004753 textile Substances 0.000 claims abstract description 9
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 claims description 48
- 239000004642 Polyimide Substances 0.000 claims description 20
- 238000007747 plating Methods 0.000 claims description 20
- 229920001721 polyimide Polymers 0.000 claims description 20
- 210000002268 wool Anatomy 0.000 claims description 20
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 16
- 238000004140 cleaning Methods 0.000 claims description 15
- 238000013033 photocatalytic degradation reaction Methods 0.000 claims description 14
- 239000000178 monomer Substances 0.000 claims description 13
- 238000006116 polymerization reaction Methods 0.000 claims description 13
- PIBWKRNGBLPSSY-UHFFFAOYSA-L palladium(II) chloride Chemical compound Cl[Pd]Cl PIBWKRNGBLPSSY-UHFFFAOYSA-L 0.000 claims description 12
- 239000002253 acid Substances 0.000 claims description 11
- 238000011065 in-situ storage Methods 0.000 claims description 11
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- 230000004913 activation Effects 0.000 claims description 9
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 8
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 8
- 239000010936 titanium Substances 0.000 claims description 8
- 229910052719 titanium Inorganic materials 0.000 claims description 8
- 238000007788 roughening Methods 0.000 claims description 6
- KWSLGOVYXMQPPX-UHFFFAOYSA-N 5-[3-(trifluoromethyl)phenyl]-2h-tetrazole Chemical compound FC(F)(F)C1=CC=CC(C2=NNN=N2)=C1 KWSLGOVYXMQPPX-UHFFFAOYSA-N 0.000 claims description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 5
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 5
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 claims description 5
- 229940040526 anhydrous sodium acetate Drugs 0.000 claims description 5
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 5
- 230000036571 hydration Effects 0.000 claims description 5
- 238000006703 hydration reaction Methods 0.000 claims description 5
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 claims description 5
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 claims description 5
- 229910017604 nitric acid Inorganic materials 0.000 claims description 5
- 239000001509 sodium citrate Substances 0.000 claims description 5
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 claims description 5
- 229910001379 sodium hypophosphite Inorganic materials 0.000 claims description 5
- 238000002604 ultrasonography Methods 0.000 claims description 5
- 230000003213 activating effect Effects 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 3
- 229960005196 titanium dioxide Drugs 0.000 claims 3
- 235000010215 titanium dioxide Nutrition 0.000 claims 3
- 239000002019 doping agent Substances 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 17
- 238000000576 coating method Methods 0.000 abstract description 14
- 230000015556 catabolic process Effects 0.000 abstract description 8
- 238000006731 degradation reaction Methods 0.000 abstract description 8
- 230000008569 process Effects 0.000 abstract description 7
- 238000012545 processing Methods 0.000 abstract description 4
- 230000007613 environmental effect Effects 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 238000004043 dyeing Methods 0.000 abstract description 2
- 239000002351 wastewater Substances 0.000 abstract description 2
- 239000003054 catalyst Substances 0.000 description 19
- 239000004065 semiconductor Substances 0.000 description 16
- 238000002835 absorbance Methods 0.000 description 14
- 239000000975 dye Substances 0.000 description 12
- 230000001699 photocatalysis Effects 0.000 description 12
- 239000000126 substance Substances 0.000 description 12
- 239000011248 coating agent Substances 0.000 description 11
- 238000004042 decolorization Methods 0.000 description 11
- 238000005516 engineering process Methods 0.000 description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 7
- RBTBFTRPCNLSDE-UHFFFAOYSA-N 3,7-bis(dimethylamino)phenothiazin-5-ium Chemical compound C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 RBTBFTRPCNLSDE-UHFFFAOYSA-N 0.000 description 6
- 238000006243 chemical reaction Methods 0.000 description 6
- 229960000907 methylthioninium chloride Drugs 0.000 description 6
- 239000002245 particle Substances 0.000 description 6
- 230000008859 change Effects 0.000 description 5
- 239000007788 liquid Substances 0.000 description 5
- 238000007146 photocatalysis Methods 0.000 description 5
- 239000001044 red dye Substances 0.000 description 5
- 238000011160 research Methods 0.000 description 5
- 239000006228 supernatant Substances 0.000 description 5
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 5
- 229910001868 water Inorganic materials 0.000 description 5
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 239000002105 nanoparticle Substances 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 3
- 238000006555 catalytic reaction Methods 0.000 description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
- 238000009713 electroplating Methods 0.000 description 3
- 229940107698 malachite green Drugs 0.000 description 3
- FDZZZRQASAIRJF-UHFFFAOYSA-M malachite green Chemical compound [Cl-].C1=CC(N(C)C)=CC=C1C(C=1C=CC=CC=1)=C1C=CC(=[N+](C)C)C=C1 FDZZZRQASAIRJF-UHFFFAOYSA-M 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 239000011941 photocatalyst Substances 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- 239000004094 surface-active agent Substances 0.000 description 3
- YXIWHUQXZSMYRE-UHFFFAOYSA-N 1,3-benzothiazole-2-thiol Chemical compound C1=CC=C2SC(S)=NC2=C1 YXIWHUQXZSMYRE-UHFFFAOYSA-N 0.000 description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- XUJNEKJLAYXESH-UHFFFAOYSA-N Cysteine Chemical compound SCC(N)C(O)=O XUJNEKJLAYXESH-UHFFFAOYSA-N 0.000 description 2
- 229960000583 acetic acid Drugs 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 230000008021 deposition Effects 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000012153 distilled water Substances 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 239000011964 heteropoly acid Substances 0.000 description 2
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 description 2
- 230000031700 light absorption Effects 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000003980 solgel method Methods 0.000 description 2
- 238000003911 water pollution Methods 0.000 description 2
- VCGRFBXVSFAGGA-UHFFFAOYSA-N (1,1-dioxo-1,4-thiazinan-4-yl)-[6-[[3-(4-fluorophenyl)-5-methyl-1,2-oxazol-4-yl]methoxy]pyridin-3-yl]methanone Chemical compound CC=1ON=C(C=2C=CC(F)=CC=2)C=1COC(N=C1)=CC=C1C(=O)N1CCS(=O)(=O)CC1 VCGRFBXVSFAGGA-UHFFFAOYSA-N 0.000 description 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- XFXPMWWXUTWYJX-UHFFFAOYSA-N Cyanide Chemical compound N#[C-] XFXPMWWXUTWYJX-UHFFFAOYSA-N 0.000 description 1
- 241000790917 Dioxys <bee> Species 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 241001125671 Eretmochelys imbricata Species 0.000 description 1
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 206010054949 Metaplasia Diseases 0.000 description 1
- 229910001096 P alloy Inorganic materials 0.000 description 1
- 241000287127 Passeridae Species 0.000 description 1
- 239000004952 Polyamide Substances 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 229940126678 chinese medicines Drugs 0.000 description 1
- 238000005253 cladding Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000001351 cycling effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 229940078469 dl- cysteine Drugs 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- 239000010881 fly ash Substances 0.000 description 1
- 239000012362 glacial acetic acid Substances 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000001802 infusion Methods 0.000 description 1
- 229910001410 inorganic ion Inorganic materials 0.000 description 1
- 230000001678 irradiating effect Effects 0.000 description 1
- 239000004310 lactic acid Substances 0.000 description 1
- 235000014655 lactic acid Nutrition 0.000 description 1
- -1 magnetism Substances 0.000 description 1
- 230000005389 magnetism Effects 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 230000015689 metaplastic ossification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 239000004570 mortar (masonry) Substances 0.000 description 1
- 239000002114 nanocomposite Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- MUJIDPITZJWBSW-UHFFFAOYSA-N palladium(2+) Chemical compound [Pd+2] MUJIDPITZJWBSW-UHFFFAOYSA-N 0.000 description 1
- 150000004968 peroxymonosulfuric acids Chemical class 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- OFNHPGDEEMZPFG-UHFFFAOYSA-N phosphanylidynenickel Chemical compound [P].[Ni] OFNHPGDEEMZPFG-UHFFFAOYSA-N 0.000 description 1
- 229920002647 polyamide Polymers 0.000 description 1
- 150000003071 polychlorinated biphenyls Chemical class 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- AKHNMLFCWUSKQB-UHFFFAOYSA-L sodium thiosulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=S AKHNMLFCWUSKQB-UHFFFAOYSA-L 0.000 description 1
- 235000019345 sodium thiosulphate Nutrition 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- YJVUGDIORBKPLC-UHFFFAOYSA-N terbium(3+);trinitrate Chemical compound [Tb+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O YJVUGDIORBKPLC-UHFFFAOYSA-N 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- ZWYDDDAMNQQZHD-UHFFFAOYSA-L titanium(ii) chloride Chemical compound [Cl-].[Cl-].[Ti+2] ZWYDDDAMNQQZHD-UHFFFAOYSA-L 0.000 description 1
- 229940034610 toothpaste Drugs 0.000 description 1
- 239000000606 toothpaste Substances 0.000 description 1
- 229910000314 transition metal oxide Inorganic materials 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 239000003403 water pollutant Substances 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
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/26—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24
- B01J31/38—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24 of titanium, zirconium or hafnium
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/30—Nature of the water, waste water, sewage or sludge to be treated from the textile industry
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Health & Medical Sciences (AREA)
- Inorganic Chemistry (AREA)
- Toxicology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Catalysts (AREA)
Abstract
The present invention relates to a kind of based on composite electroless-plating fiber base nickel-loaded/optically catalytic TiO 2 degradable material preparation method, including：The preparation of polyaniline fabric, palladium activated textile, Composite Coatings nickel/titanium dioxide fabric.Present invention process is easy, low in cost, high production efficiency, environmental protection and energy saving；The composite electroless-plating nickel/titanium dioxide textile flexibility of preparation is good, reusable, and has excellent degradation capability, can be widely applied to the processing of dyeing waste water.
Description
Technical field
The invention belongs to fabric functional method for sorting fields, in particular to a kind of to be loaded based on composite electroless-plating fiber base
The preparation method of nickel/titanium dioxide photocatalytic degradation material.
Background technique
Composite chemical coating technology starts to develop in states such as early 1970s moral, Japan and the United States, obtains in the industry to today
Existing more than 40 years history is widely applied.Composite electroless-plating is an important directions of Composite Plating, is the side with chemical plating
Method makes solid particle and technique of the metal co-deposition to obtain composite deposite.Electroless nanometer composite coating be by nanoscale not
Molten particle replaces the particle of micro-meter scale and matrix metal to be co-deposited to matrix surface.Electroless nanometer composite coating has become multiple at present
Close a kind of development trend of chemical plating.This composite deposite has superior performance, Er Qieyou than micron particles composite deposite
In the introducing of nano particle, it is also possible to the exceptional function with some nano materials.Grinding in relation to electroless nanometer composite coating at present
Study carefully as follows, Shen Yue army of Guizhou University is to nickel phosphorus (Ni-P)-nano-titanium dioxide (TiO2) composite electroless-plating complexant ground
Study carefully, has studied the influence of three kinds of citric acid, lactic acid and amion acetic acid complexants to plating solution and coating performance.Guizhou University's chemistry with
Chemical science school relaxes using bath stability, deposition rate, plating layer porosity, microhardness and corrosion resistance as evaluation index, research
Three kinds of sodium thiosulfate, 2-mercaptobenzothiazole and DL-cysteine stabilizers are to Ni-P nano-TiO2Composite electroless-plating
Influence.HeFei University of Technology Qian Lihua has primarily determined Ni-P-TiO using orthogonal experiment2Electroless nanometer composite coating technique
Basic recipe.Have studied the influence and nanoparticle of mixing speed, surfactant additional amount, pH value, temperature to deposition velocity
The influence of sub- additional amount, agitating mode, mixing speed, kinds of surfactants to coating Nanocomposites amount obtains best
Process recipe.Northeast Petroleum University's machine science and engineering college family will space use fluorine carbocation type surfactant and ultrasound
Wave technology is pre-dispersed to nanoparticle progress, and chemical plating Mi-P alloy plating solution is added and is prepared for Ni-P- nano-TiO2Composite deposite,
And obtain different technical parameters to the affecting laws of nanoparticle content in chemical deposit by grouping experiment.
Titanium dioxide (TiO2) it is a kind of very important transition metal oxide, work is achieved that early in earlier 1900s
Industry metaplasia produces, and is widely used in the industries such as toothpaste, paint, coating.1972, Honda and Fujishima were in TiO2Electrode
On have found photocatalytic water generate H2The phenomenon that, it has risen within the scope of global boundary to TiO later2Research boom.1976, Carey
Etc. reporting TiO2Make the research of Polychlorinated biphenyls dealuminated USY cataluyst under black light, to open TiO2In photocatalytic degradation dirt
Contaminate the application in object space face.Bard in 1997 and Frank et al. are by TiO2It is relatively early by dioxy applied to the degradation of cyanide in water
Change the example that titanium is used for water pollutant processing.Currently, the TiO of different shape structure2Nano material oneself show in different field
Respective huge application potential out, and cheap, stable, high performance semiconductor catalyst is the basis of photocatalysis technology, in crowd
In more semiconductor light-catalysts, TiO2Photochemical catalyst is easy to operate, less energy consumption, degradation range is wide, degradation speed is fast, at low cost
Honest and clean, excellent photocatalysis performance becomes one of most promising semiconductor light-catalyst.
Now, Green Chemical Technology has huge potentiality in terms of reducing energy consumption, it will promote environment and warp
Ji is coordinated, and social sustainable development is pushed, and being catalyzed is one of Green Chemistry key technology.Light-catalyzed reaction be light and substance it
Between one of the various ways that interact, be the unification of light reaction and catalysis reaction, be the institute under light and catalyst simultaneously effect
The chemical reaction of progress.Currently, environmental problem and energy problem are facing mankinds and two significant problems must solving, and light
Catalysis technique is due to its cleaning and can directly utilize the characteristic of solar energy, and becomes ideal environmental pollution improvement and clean energy resource
Production technology.
Photocatalysis can be used for generating hydrogen by photocatalytic water splitting as a kind of green photo chemistry technology newly developed,
It can also be used for for organic pollutant being oxidized to water, carbon dioxide and inorganic ions.Photocatalysis technology is a kind of special based on semiconductor
A kind of technology that different band structure is established, core are semiconductor light-catalysts.The energy band of semiconductor is occupied by electronics
The low energy valence band and electronics of track do not occupy composed by the higher energy conduction band of track composition, deposit between the valence band and conduction band of semiconductor
In forbidden band, the size of forbidden band is known as forbidden bandwidth between valence band and conduction band.Photocatalytic process based on semiconductor mainly includes three
A step：1. being greater than or equal on the solar radiation to semiconductor of semiconductor forbidden bandwidth, semiconductor excitation generates photoproduction and carries
Stream；2. photo-generated carrier is compound, separates and move to the surface of semiconductor light-catalyst；3. migrating to the light of semiconductor surface
The different plant species that raw carrier will be adsorbed with catalyst surface react, move to the photo-generated carrier of semiconductor surface with
The substance reaction of photocatalyst surface absorption.
Traditional photocatalysis is administered water pollution and is generally carried out in suspension phase system, although the disposal efficiency is high, because of powder
Particle is tiny, recycles highly difficult, easily outflows with water and wastes, thus catalyst is fixed and recovery technology receive it is considerable degree of
Concern.There is research that catalyst is fixed on the carriers such as magnetism, flyash, making it not only has preferable photocatalytic activity, but also energy
Multiple cycling and reutilization.But the research of fiber base loaded optic catalyst is also rarely reported at present, composite electroless-plating in this approach
Fiber base nickel-loaded/optically catalytic TiO 2 degradable material has not been reported yet.
Summary of the invention
Technical problem to be solved by the invention is to provide one kind to load nickel/titanium dioxide based on composite electroless-plating fiber base
The preparation method of photocatalytic degradation material, the disposal efficiency is low when overcoming prior art photochemical catalyst to administer water pollution, recycling
Difficulty, the defect that cannot be repeatedly used.
Of the invention is a kind of based on composite electroless-plating fiber base nickel-loaded/optically catalytic TiO 2 degradable material preparation side
Method, including：
(1) fabric is first subjected to cleaning roughening, then with bath raio for 1:40~50 are placed in aniline monomer doping acid solution,
Ammonium persulfate is added and carries out in-situ polymerization, is washed to neutrality, dries, obtain polyaniline fabric, wherein aniline monomer and persulfuric acid
The molar ratio of ammonium is 0.15~0.55:0.15~0.55；
(2) polyaniline fabric in step (1) is placed in palladium chloride activating solution and is activated, obtain palladium activated textile, then with
Bath raio is 1:40~50 are impregnated in plating solution, carry out composite electroless-plating nickel/titanium dioxide, obtain fiber base nickel-loaded/titanium dioxide
Titanium photocatalytic degradation material.
Fabric is polyimides fabric or wool fabric in the step (1).
The fabric is polyimides fabric, and cleaning is specially：Polyimides fabric is placed in 4~16g/L sodium hydroxide
In solution, 5~25min is kept at 60~100 DEG C.
The fabric is wool fabric, and cleaning is specially：Wool fabric is placed in 20~40min of ultrasound in dehydrated alcohol.
Aniline monomer doping acid solution is in the step (1)：0.15~0.55mol/L aniline, 0.35~0.75mol/L
Nitric acid.
The time being placed in aniline monomer doping acid solution in the step (1) is 20~60min.
Original position polymerization temperature is 15~25 DEG C in the step (1), and the in-situ polymerization time is 1.5~4.5h；Dry temperature
It is 10~40 DEG C, flash-off time is 3~7h.
Palladium chloride activation solution concentration is 0.5~1.25g/L in the step (2).
Plating solution is in the step (2)：20~60g/L of six hydration nickel sulfate, 5~25g/L of sodium citrate, sodium hypophosphite
20~60g/L, 5~25g/L of anhydrous sodium acetate, 1~3g/L of nano-titanium dioxide, 40~80 DEG C of temperature, pH value 4~8.
Activation time is 0.5~3.5h in the step (2)；The time of composite electroless-plating is 1~3h.
Beneficial effect
The present invention uses composite chemical electroplating method, simple process, low in cost, high production efficiency, environmental protection and energy saving；The present invention
Prepared composite electroless-plating nickel/titanium dioxide fabric coating even compact, binding force of cladding material is good, has excellent photocatalytic
Can, the dye decolored rate of wool fabric obtained is 95% or more, and polyimides dye for fabrics percent of decolourization obtained is 85% or more.
Heteropolyacid catalyst β-the SiW of semiconductor titanium dichloride load prepared by comparative example 112/TiO2To methylene blue in natural lighting
Lower 2.5h is penetrated, percent of decolourization reaches 86.79%；Tb prepared by comparative example 23+-TiO2Photochemical catalyst is degraded hole under natural light irradiation
Sparrow malachite green solution 3h, for percent of decolourization up to 81.1%, the percent of decolourization of the two is suitable with the present invention, but the two is not loaded to and knitted
On object, it is unsatisfactory for repeatedly using.To sum up compound material flexible prepared by the present invention is good, reusable, can be widely applied
In the processing of dyeing waste water.
Detailed description of the invention
Fig. 1 is composite electroless-plating schematic diagram of the present invention and dye liquor photocatalytic degradation figure；Wherein, 1 is original fabrics；2 be poly-
Aniline fabric；3 be composite nickel-plating-titanium dioxide fabric；4 be dye liquor before photocatalytic degradation；5 be dye liquor after photocatalytic degradation；①
For ultraviolet or visible light conditions.
Fig. 2 is wool fabric surface scan electron microscope in embodiment 1；Wherein, a is as former state；B is cleaning sample；C is poly- for aniline
Close processing sample；D is composite nickel-plating/titanium dioxide treatment sample.
Fig. 3 is polyimides fabric surface scanning electron microscope (SEM) photograph in embodiment 2；Wherein, a is as former state；B is cleaning roughening sample；c
Sample is handled for aniline polymerization；D is composite nickel-plating/titanium dioxide treatment sample.
Fig. 4 is the absorbance of wool fabric and non-sorting wool fabric after arrangement in embodiment 1 with the variation of irradiation time
Figure.
Fig. 5 is polyimides fabric and when not arranging the absorbance of polyimides fabric with irradiating after arranging in embodiment 2
Between variation diagram.
Specific embodiment
Present invention will be further explained below with reference to specific examples.It should be understood that these embodiments are merely to illustrate the present invention
Rather than it limits the scope of the invention.In addition, it should also be understood that, after reading the content taught by the present invention, those skilled in the art
Member can make various changes or modifications the present invention, and such equivalent forms equally fall within the application the appended claims and limited
Range.
In embodiment, the wool grammes per square metre used is 370g/m2, the polyimides grammes per square metre used is 250g/m2, hydrogen-oxygen used
Change sodium be purchased from Pinghu chemical reagent factory, titanium dioxide used be purchased from Shanghai Mike woods biochemical technology Co., Ltd, anhydrous sodium acetate,
Aniline, nitric acid, ammonium persulfate, palladium chloride, six hydration nickel sulfate, sodium citrate, sodium hypophosphite are purchased from Chinese medicines group chemistry
Reagent Co., Ltd.Other reagents are that analysis is pure, in use without further purification.
Embodiment 1
In-situ polymerization aniline after wool cleaning, palladium chloride activation, plates to obtain nickel/bis- using composite chemical electroplating method on wool
Titanium coating is aoxidized, is then irradiated under ultraviolet or visible light.The specific steps are that：
(1) clip 4cm × 4cm wool fabric, ultrasound 35min in dehydrated alcohol；Wool fabric after cleaning is placed in benzene
Amine monomers adulterate 45min in acid solution, bath raio 1：50, aniline monomer adulterates acid solution and is：0.35mol/L aniline, 0.7mol/L
Nitric acid；Ammonium persulfate (concentration of ammonium persulfate in the solution is 0.35mol/L) in-situ polymerization 3.5h at 20 DEG C, washing is added
To neutrality, is dried at 20 DEG C by 4 hours, obtain polyaniline fabric.
(2) polyaniline fabric is placed in palladium chloride activating solution (palladium chloride activation solution concentration is 0.8g/L) and activates 0.5h,
Obtain palladium activated textile.Palladium activated textile is impregnated in composite electroless-plating 2h in plating solution, bath raio 1：50, plating solution is：Six hydrations
Nickel sulfate 30g/L, sodium citrate 6g/L, sodium hypophosphite 28g/L, anhydrous sodium acetate 8g/L, temperature 70 C, pH value 5, nanometer two
Titanium oxide 1.2g/L；Obtain Composite Coatings nickel/titanium dioxide fabric.
(3) 50mg/L active red dye liquor is prepared respectively and be placed in 50mL in beaker, then respectively by composite nickel-plating/titanium dioxide
Titanium fabric and unfinished wool fabric are placed in a beaker, and 2.5h are irradiated under ultraviolet or visible light, the absorbance of fabric is with photograph
The variation of time is penetrated as shown in figure 4, the dye decolored rate of wool fabric is as shown in table 1 after arranging.
Fig. 4 shows：Wool is very little to the absorption of active red dye liquor, and nickel-loaded-titanium dioxide wool fabric is to dye
The photocatalytic degradation effect of liquid is significant, with light application time increase absorbance be near linear downward trend, 140 minutes with
Absorbance is reduced to 0.05 afterwards, and dye liquor has excellent photocatalytic degradation close to clear, composite nickel-plating-titanium dioxide wool fabric
Ability.
Embodiment 2
In-situ polymerization aniline after polyimides cleaning roughening, palladium chloride activation, using composite chemical electroplating method in polyamides Asia
Nickel/titanium dioxide coating is plated to obtain on amine, is then irradiated under ultraviolet or visible light.The specific steps are that：
(1) clip 4cm × 5cm polyimides fabric prepares the sodium hydroxide solution of 10g/L, and 85 DEG C are knitted polyimides
Object carries out cleaning roughening 15min；Fabric after cleaning roughening is placed in 45min in aniline monomer doping acid solution, bath raio 1：45,
Aniline monomer adulterates acid solution：0.25mol/L aniline, 0.5mol/L nitric acid；Ammonium persulfate is added, and (ammonium persulfate is in the solution
Concentration be 0.25mol/L) the in-situ polymerization 1.5h at 20 DEG C, be washed to neutrality, dry, obtain by 4 hours at 20 DEG C
Polyaniline fabric.
(2) polyaniline fabric is placed in palladium chloride activating solution (palladium chloride concentration is 1g/L) and activates 1.5h, it is living to obtain palladium
Change fabric.Palladium activated textile is impregnated in composite electroless-plating 1.5h in plating solution, bath raio 1：50, plating solution is：Six hydration nickel sulfate
35g/L, sodium citrate 7g/L, sodium hypophosphite 32g/L, anhydrous sodium acetate 8g/L, 80 DEG C of temperature, pH value 6, nano-titanium dioxide
1.2g/L；Obtain Composite Coatings nickel/titanium dioxide fabric.
(3) 50mg/L active red dye liquor is prepared respectively and be placed in 50mL in beaker, then respectively by composite nickel-plating/titanium dioxide
Titanium fabric and unfinished polyimides fabric are placed in a beaker, and irradiate 2h under ultraviolet or visible light, the absorbance of fabric with
The variation of irradiation time is as shown in figure 5, the dye decolored rate of polyimides fabric is as shown in table 1 after arranging.
Fig. 1 shows entire composite electroless-plating process and photocatalytic degradation of dye process.It can be expressed as the fabric after cleaning
It is placed in aniline monomer doping acid solution, carries out in-situ polymerization, obtain polyaniline fabric；Polyaniline fabric is placed in palladium chloride activation
In liquid, it is palladium atom activation site that polyaniline, which restores palladium ion, obtains palladium activated textile；Palladium activated textile is impregnated in composite plating bath
In, composite electroless-plating nickel/titanium dioxide is carried out later, obtains fiber base nickel-loaded/optically catalytic TiO 2 fabric；It finally will preparation
It is that a few hours degradation is irradiated under ultraviolet or visible light in 50mg/L active red dye liquor that good fabric, which is placed in 50mL concentration,.
Fig. 2 and Fig. 3 show：A, which can see, in figure adheres to some spots on fiber；B, which can see, to be attached on fiber
Greasiness removal；C can see aniline on fiber and fibre gap in-situ polymerization, wrap up fiber；D can be seen that nano-silica
Change titanium particle to be evenly distributed in nickel metal layer.
Fig. 5 shows：Polyimides almost can be ignored the absorption of active red dye liquor, nickel-loaded-titanium dioxide
Polyimides fabric is significant to the photocatalytic degradation effect of dye liquor, as the increase absorbance of light application time is approximate with light application time
Negative correlation, absorbance is reduced to 0.09 after 140 minutes, and dye liquor is close to be clarified, composite nickel-plating-titanium dioxide polyimides
Fabric has preferable photocatalytic degradation capability.
Table 1
| Fabric | Wool | Polyimides |
| Percent of decolourization (η) | 95% | 85% |
Comparative example 1
β-SiW is synthesized using infusion process first12And TiO2Composite catalyst β-SiW12/TiO2, and study under different condition
The ability of catalyst degradation methylene blue.(semiconductor titanium dioxide is prepared referring to Qiqihar City Environment Monitoring Central Station Ma Xuguang
Heteropolyacid catalyst β-the SiW of titanium load12/TiO2)
1.β-SiW12/TiO2Influence of the dosage to photocatalytic activity
The methylene blue solution for measuring 50mL30mg/L respectively pours into 5 small beakers, and β-SiW12/TiO is respectively added2It urges
It is protected from light absorption 50min after agent 6mg, 8mg, 10mg, 12mg, 14mg, ultrasonic 5min, supernatant liquor is taken to measure it at 664nm
Absorbance.Then it being placed under ultraviolet lamp again and irradiates 150min, interval 15min takes supernatant liquor to survey its absorbance value at 664nm,
Calculate percent of decolourization.β-SiW12/TiO2Amount when being 12mg percent of decolourization it is maximum, can reach 82.83%.
2. influence of the solution ph to photocatalytic activity
The methylene blue of 50mL30mg/L is measured respectively in 5 beakers, and solution ph is adjusted to 2,4,6,8 and respectively
10, each β-SiW that 12mg is added12/TiO2, under the conditions of ultraviolet light irradiation 150min, interval 15min takes supernatant liquor in 664nm
Place surveys its absorbance value, calculates percent of decolourization.When the pH value of solution is 6, percent of decolourization maximum is up to 82.83%.
3. the influence that different light sources degrade to methylene blue
The methylene blue solution pH value for adjusting 30mg/L is 6, surveys its absorbance, takes 3 parts, is separately added into the β-of 12mg
SiW12/TiO2, carried out after ultrasound is protected from light absorption 50min, wherein 1 part is placed under natural light and irradiates 150min, 1 part
150min is irradiated under 15W ultraviolet lamp, 1 part is protected from light 150min, take a certain amount of supernatant liquor every 15min respectively, 664nm most
Absorbance is measured under big absorbing wavelength, calculates solution percent of decolourization, sunlight irradiates lower percent of decolourization and reaches 86.79%.
Comparative example 2
Tb is prepared using sol-gel method3+Doped nanometer titanium dioxide photocatalyst is (quiet referring to packet header college of education Liu Li
Et al. using sol-gel method synthesize Tb3+-TiO2Photochemical catalyst), solution A is prepared respectively：Suitable terbium nitrate solution is taken (to make
Tb3+-TiO2Molar ratio be 2.5%) be added to bis- glacial acetic acid of 9ml, 40ml dehydrated alcohol and 10ml distilled water composition mixing
In liquid；Solution B：The butyl titanate of 20mI is uniformly mixed with 50mI dehydrated alcohol；Solution B is added dropwise to vigorous stirring molten
In liquid A, after being added dropwise, continues to stir 3h, be then placed at room temperature for into gel.Gel in beaker, then it is placed on dry
(80 DEG C) drying in dry case, are crushed into powder shape after drying with mortar, finally after 5RJX4-13 Muffle kiln roasting 3h again
Grinding finally obtains target product Tb3+Doped nanometer titanium dioxide photocatalyst.
Under natural light irradiation, the stirring at normal temperature in constant temperature blender with magnetic force, reaction starts rear timing, takes every 30min
Sample is primary, samples six times altogether, is centrifugated with 3500r/min and removes catalyst granules, taken supernatant, do reference with distilled water
Liquid, in Vis-7220 visible spectrophotometer (λmax=616nm) measurement reaction solution absorbance, urged with the light of test sample
Change performance.Work as Tb3+Doping is 2.5%, and photocatalytic degradation malachite green effect is best at 400 DEG C, degrading malachite green solution
3h, degradation rate is up to 81.1%.
Claims (10)
1. it is a kind of based on composite electroless-plating fiber base nickel-loaded/optically catalytic TiO 2 degradable material preparation method, including：
(1) fabric is first subjected to cleaning roughening, then with bath raio for 1:40~50 are placed in aniline monomer doping acid solution, are added
Ammonium persulfate carries out in-situ polymerization, be washed to neutrality, dry, obtain polyaniline fabric, wherein aniline monomer and ammonium persulfate
Molar ratio is 0.15~0.55:0.15~0.55；
(2) polyaniline fabric in step (1) is placed in palladium chloride activating solution and is activated, palladium activated textile is obtained, then with bath raio
It is 1:40~50 are impregnated in plating solution, carry out composite electroless-plating nickel/titanium dioxide, obtain fiber base nickel-loaded/titanium-dioxide photo
Catalytic degradation material.
2. preparation method according to claim 1, which is characterized in that fabric is polyimides fabric in the step (1)
Or wool fabric.
3. preparation method according to claim 2, which is characterized in that the fabric is polyimides fabric, and cleaning is specific
For：Polyimides fabric is placed in 4~16g/L sodium hydroxide solution, 5~25min is kept at 60~100 DEG C.
4. preparation method according to claim 2, which is characterized in that the fabric is wool fabric, and cleaning is specially：It will
Wool fabric is placed in 20~40min of ultrasound in dehydrated alcohol.
5. preparation method according to claim 1, which is characterized in that aniline monomer adulterates acid solution in the step (1)
For：
0.15~0.55mol/L aniline, 0.35~0.75mol/L nitric acid.
6. preparation method according to claim 1, which is characterized in that be placed in aniline monomer dopant acid in the step (1)
Time in solution is 20~60min.
7. preparation method according to claim 1, which is characterized in that in the step (1) in situ polymerization temperature be 15~
25 DEG C, the in-situ polymerization time is 1.5~4.5h；Drying temperature is 10~40 DEG C, and flash-off time is 3~7h.
8. preparation method according to claim 1, which is characterized in that palladium chloride activation solution concentration is in the step (2)
0.5~1.25g/L.
9. preparation method according to claim 1, which is characterized in that plating solution is in the step (2)：Six hydration nickel sulfate
20~60g/L, 5~25g/L of sodium citrate, 20~60g/L of sodium hypophosphite, 5~25g/L of anhydrous sodium acetate, nanometer titanium dioxide
1~3g/L of titanium, 40~80 DEG C of temperature, pH value 4~8.
10. preparation method according to claim 1, which is characterized in that in the step (2) activation time be 0.5~
3.5h；
The time of composite electroless-plating is 1~3h.
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