CN110156118A - A kind of Combined electrode and its preparation method and application - Google Patents
A kind of Combined electrode and its preparation method and application Download PDFInfo
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- CN110156118A CN110156118A CN201910302264.5A CN201910302264A CN110156118A CN 110156118 A CN110156118 A CN 110156118A CN 201910302264 A CN201910302264 A CN 201910302264A CN 110156118 A CN110156118 A CN 110156118A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- RAXXELZNTBOGNW-UHFFFAOYSA-N imidazole Natural products C1=CNC=N1 RAXXELZNTBOGNW-UHFFFAOYSA-N 0.000 claims abstract description 64
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 56
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 46
- 239000002041 carbon nanotube Substances 0.000 claims abstract description 42
- 229910021393 carbon nanotube Inorganic materials 0.000 claims abstract description 41
- 239000002071 nanotube Substances 0.000 claims abstract description 28
- DHRLEVQXOMLTIM-UHFFFAOYSA-N phosphoric acid;trioxomolybdenum Chemical compound O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.OP(O)(O)=O DHRLEVQXOMLTIM-UHFFFAOYSA-N 0.000 claims abstract description 28
- 239000007788 liquid Substances 0.000 claims abstract description 24
- 230000020477 pH reduction Effects 0.000 claims abstract description 24
- 239000011159 matrix material Substances 0.000 claims abstract description 19
- 125000005575 polycyclic aromatic hydrocarbon group Chemical group 0.000 claims abstract description 17
- 238000000151 deposition Methods 0.000 claims abstract description 10
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 41
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 37
- 239000008367 deionised water Substances 0.000 claims description 29
- 229910021641 deionized water Inorganic materials 0.000 claims description 29
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical group [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 22
- 238000000034 method Methods 0.000 claims description 18
- 239000003792 electrolyte Substances 0.000 claims description 17
- 150000002500 ions Chemical class 0.000 claims description 15
- -1 fluoride ion compound Chemical class 0.000 claims description 12
- 229910052697 platinum Inorganic materials 0.000 claims description 11
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 9
- 229910017604 nitric acid Inorganic materials 0.000 claims description 9
- 238000002484 cyclic voltammetry Methods 0.000 claims description 8
- 229910052719 titanium Inorganic materials 0.000 claims description 8
- 239000010936 titanium Substances 0.000 claims description 8
- 230000000593 degrading effect Effects 0.000 claims description 7
- 238000007743 anodising Methods 0.000 claims description 6
- 229940075397 calomel Drugs 0.000 claims description 6
- ZOMNIUBKTOKEHS-UHFFFAOYSA-L dimercury dichloride Chemical compound Cl[Hg][Hg]Cl ZOMNIUBKTOKEHS-UHFFFAOYSA-L 0.000 claims description 6
- 238000006555 catalytic reaction Methods 0.000 claims description 5
- 238000006243 chemical reaction Methods 0.000 claims description 5
- 239000000758 substrate Substances 0.000 claims description 5
- 230000004913 activation Effects 0.000 claims description 4
- 230000008569 process Effects 0.000 claims description 4
- 238000001802 infusion Methods 0.000 claims description 3
- 239000002608 ionic liquid Substances 0.000 claims description 3
- 239000002253 acid Substances 0.000 claims description 2
- 150000001298 alcohols Chemical class 0.000 claims description 2
- 238000001354 calcination Methods 0.000 claims description 2
- 238000011065 in-situ storage Methods 0.000 claims description 2
- 239000000463 material Substances 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- AMWVZPDSWLOFKA-UHFFFAOYSA-N phosphanylidynemolybdenum Chemical compound [Mo]#P AMWVZPDSWLOFKA-UHFFFAOYSA-N 0.000 claims description 2
- 229920006395 saturated elastomer Polymers 0.000 claims description 2
- 239000004408 titanium dioxide Substances 0.000 claims 2
- 230000005611 electricity Effects 0.000 claims 1
- 238000006731 degradation reaction Methods 0.000 abstract description 9
- 230000015556 catabolic process Effects 0.000 abstract description 8
- 238000005516 engineering process Methods 0.000 abstract description 3
- 239000000243 solution Substances 0.000 description 15
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 12
- YNPNZTXNASCQKK-UHFFFAOYSA-N phenanthrene Chemical compound C1=CC=C2C3=CC=CC=C3C=CC2=C1 YNPNZTXNASCQKK-UHFFFAOYSA-N 0.000 description 12
- 230000003647 oxidation Effects 0.000 description 11
- 238000007254 oxidation reaction Methods 0.000 description 11
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 7
- 238000004140 cleaning Methods 0.000 description 7
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 6
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 6
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 6
- 230000008021 deposition Effects 0.000 description 6
- 238000002604 ultrasonography Methods 0.000 description 6
- 229910052799 carbon Inorganic materials 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 235000019441 ethanol Nutrition 0.000 description 5
- DDFHBQSCUXNBSA-UHFFFAOYSA-N 5-(5-carboxythiophen-2-yl)thiophene-2-carboxylic acid Chemical compound S1C(C(=O)O)=CC=C1C1=CC=C(C(O)=O)S1 DDFHBQSCUXNBSA-UHFFFAOYSA-N 0.000 description 4
- 239000007864 aqueous solution Substances 0.000 description 4
- 150000001875 compounds Chemical class 0.000 description 4
- 150000003254 radicals Chemical class 0.000 description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 3
- 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 3
- 239000012901 Milli-Q water Substances 0.000 description 3
- 244000137852 Petrea volubilis Species 0.000 description 3
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 3
- LDDQLRUQCUTJBB-UHFFFAOYSA-N ammonium fluoride Chemical group [NH4+].[F-] LDDQLRUQCUTJBB-UHFFFAOYSA-N 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- BNIILDVGGAEEIG-UHFFFAOYSA-L disodium hydrogen phosphate Chemical compound [Na+].[Na+].OP([O-])([O-])=O BNIILDVGGAEEIG-UHFFFAOYSA-L 0.000 description 3
- 229910000397 disodium phosphate Inorganic materials 0.000 description 3
- 235000019800 disodium phosphate Nutrition 0.000 description 3
- 238000005265 energy consumption Methods 0.000 description 3
- 239000011888 foil Substances 0.000 description 3
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- 239000001257 hydrogen Substances 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 238000005498 polishing Methods 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- 239000011734 sodium Substances 0.000 description 3
- 229910052708 sodium Inorganic materials 0.000 description 3
- 239000001488 sodium phosphate Substances 0.000 description 3
- KXCVJPJCRAEILX-UHFFFAOYSA-M 1-butyl-3-methylimidazol-3-ium;hydrogen sulfate Chemical compound OS([O-])(=O)=O.CCCCN1C=C[N+](C)=C1 KXCVJPJCRAEILX-UHFFFAOYSA-M 0.000 description 2
- UFWIBTONFRDIAS-UHFFFAOYSA-N Naphthalene Chemical compound C1=CC=CC2=CC=CC=C21 UFWIBTONFRDIAS-UHFFFAOYSA-N 0.000 description 2
- 229910020881 PMo12O40 Inorganic materials 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 238000009825 accumulation Methods 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 150000002460 imidazoles Chemical class 0.000 description 2
- 230000002688 persistence Effects 0.000 description 2
- BBEAQIROQSPTKN-UHFFFAOYSA-N pyrene Chemical compound C1=CC=C2C=CC3=CC=CC4=CC=C1C2=C43 BBEAQIROQSPTKN-UHFFFAOYSA-N 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- FHDQNOXQSTVAIC-UHFFFAOYSA-M 1-butyl-3-methylimidazol-3-ium;chloride Chemical compound [Cl-].CCCCN1C=C[N+](C)=C1 FHDQNOXQSTVAIC-UHFFFAOYSA-M 0.000 description 1
- 241000790917 Dioxys <bee> Species 0.000 description 1
- HGWOWDFNMKCVLG-UHFFFAOYSA-N [O--].[O--].[Ti+4].[Ti+4] Chemical compound [O--].[O--].[Ti+4].[Ti+4] HGWOWDFNMKCVLG-UHFFFAOYSA-N 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- 238000011953 bioanalysis Methods 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000001627 detrimental effect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000037213 diet Effects 0.000 description 1
- 235000005911 diet Nutrition 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- GVEPBJHOBDJJJI-UHFFFAOYSA-N fluoranthrene Natural products C1=CC(C2=CC=CC=C22)=C3C2=CC=CC3=C1 GVEPBJHOBDJJJI-UHFFFAOYSA-N 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 230000001699 photocatalysis Effects 0.000 description 1
- 238000000053 physical method Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 238000001338 self-assembly Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- JRMUNVKIHCOMHV-UHFFFAOYSA-M tetrabutylammonium bromide Chemical compound [Br-].CCCC[N+](CCCC)(CCCC)CCCC JRMUNVKIHCOMHV-UHFFFAOYSA-M 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 231100001234 toxic pollutant Toxicity 0.000 description 1
- 229910021642 ultra pure water Inorganic materials 0.000 description 1
- 239000012498 ultrapure water Substances 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- 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
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
- C02F1/461—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
- C02F1/46104—Devices therefor; Their operating or servicing
- C02F1/46109—Electrodes
-
- 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
- C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
- C02F1/461—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
- C02F1/467—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis by electrochemical disinfection; by electrooxydation or by electroreduction
- C02F1/4672—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis by electrochemical disinfection; by electrooxydation or by electroreduction by electrooxydation
-
- 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
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/725—Treatment of water, waste water, or sewage by oxidation by catalytic oxidation
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
- C25D11/02—Anodisation
- C25D11/26—Anodisation of refractory metals or alloys based thereon
-
- 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
- C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
- C02F1/461—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
- C02F1/46104—Devices therefor; Their operating or servicing
- C02F1/46109—Electrodes
- C02F2001/46133—Electrodes characterised by the material
-
- 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
- C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
- C02F1/461—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
- C02F1/46104—Devices therefor; Their operating or servicing
- C02F1/46109—Electrodes
- C02F2001/46133—Electrodes characterised by the material
- C02F2001/46138—Electrodes comprising a substrate and a coating
- C02F2001/46142—Catalytic coating
-
- 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
- C02F2101/32—Hydrocarbons, e.g. oil
Abstract
The present invention relates to photo-electrocatalytic technology fields, specifically disclose a kind of Combined electrode and its preparation method and application.The combination electrode successively includes electrode matrix, titania nanotube, acidification carbon nanotube, imidazole type ion liquid and phosphomolybdic acid from the inside to the outside, preparation method is that titania nanotube is made on electrode matrix, it will be acidified again carbon nanotube loaded on the titania nanotube, and then be sequentially depositing imidazole type ion liquid and phosphomolybdic acid.The combination electrode can efficient degradation polycyclic aromatic hydrocarbon at lower current densities.
Description
Technical field
The present invention relates to photo-electrocatalytic technology field more particularly to a kind of Combined electrode and preparation method thereof and answer
With.
Background technique
Polycyclic aromatic hydrocarbon is a kind of compound of more than two aromatic ring fusions together, it is prevalent in environment, this
Class compound is difficult to biodegrade due to poorly water-soluble, thus constantly accumulation in the environment, is that a kind of persistence difficult to degrade has
Machine object.With Chinese Industrialization, urbanization and the fast development of intensive agriculture, polycyclic aromatic hydrocarbon enters the approach of environment increasingly
Extensively, cause environmental pollution therewith to be also more and more taken seriously.Polycyclic aromatic hydrocarbon is the compound with " three cause " effect, Yi Jisheng
Object accumulation, biomagnification and persistence toxic action and be considered as environment toxic pollutant.Mainly pass through atmosphere, the side such as diet
Formula enters human body, is detrimental to health.
Polycyclic aromatic hydrocarbon has hydrophobicity, and fat-soluble larger when phenyl ring number is more, the polycyclic aromatic hydrocarbon of macromolecule can then be inhaled
It invests and enters deposit on particle, therefore polycyclic aromatic hydrocarbon is mostly the polycyclic aromatic hydrocarbon of low molecular weight, such as naphthalene, phenanthrene and pyrene in water.
Mode mainly volatilization, absorption, biodegrade and the light Fenton (UV/H of polycyclic aromatic hydrocarbon in water removal are removed at present2O2The methods of), although
Certain removal effect can be obtained to polycyclic aromatic hydrocarbon to a certain extent, however these methods all have a some shortcomings, volatilization and
The physical methods removal rates such as absorption are lower, and slowly and by such environmental effects, light Fenton can then consume chemical drugs for bioanalysis reaction
Agent makes costly and generates secondary pollution.Photoproduction can effectively be realized using the united method of photocatalysis and electrochemistry
The separation of electronics and photohole promotes the generation of free radical, to promote the degradation effect to target contaminant.Traditional light
Although electrocatalytic oxidation can remove the polycyclic aromatic hydrocarbon in water removal, to still having, low to the utilization rate of light, energy consumption is high is lacked
Point.So the method for the photoelectric catalysis degrading polycyclic aromatic hydrocarbon that research and development have high light utilization rate and low energy consumption is of great significance.
Summary of the invention
The problems such as low high with energy consumption for existing photoelectric catalysis degrading polycyclic aromatic hydrocarbon light utilization efficiency, the present invention provides a kind of new
Type combination electrode, and preparation method and application are provided.
To achieve the above object of the invention, present invention employs the following technical solutions:
A kind of Combined electrode, successively include: from the inside to the outside electrode matrix, titania nanotube, acidification carbon receive
Mitron, imidazole type ion liquid and phosphomolybdic acid.
In electrode of the present invention, using titania nanotube and acidification carbon nanotube as complex carrier, it can efficiently use
The photoelectron of visible light part in the sun, generation is efficiently transmitted on phosphomolybdic acid by carbon nanotube and imidazole type ion liquid,
Free radical is converted by photoelectron by phosphomolybdic acid；Imidazole type ion liquid has stronger affinity to phosphomolybdic acid, and has
Preferable chemical property is conducive to the catalytic performance for strengthening combination electrode.Furthermore phosphomolybdic acid can also be generated using ultraviolet light
Photoelectron generates the free radical of strong oxidizing property.A large amount of free radicals that the electrode generates can make it real at lower current densities
Now to the efficient degradation of polycyclic aromatic hydrocarbon.The caliber and length of titania nanotube and acidification carbon nanotube are multiple to this in the present invention
The performance of composite electrode is not limited thereof without significant impact.
The imidazole type ion liquid is dissolved in water, such as the inorganic acid salt etc. of 1,3- dialkyl group substituted imidazole.
Preferably, the Combined electrode is titania nanotube to be made on electrode matrix, then acidification carbon is received
Mitron is carried on the titania nanotube, is then sequentially depositing imidazole type ion liquid and phosphomolybdic acid, is made described new
Type combination electrode.
Compared with the existing technology, in combination electrode of the present invention, will be acidified it is carbon nanotube loaded on titania nanotube,
It is sequentially depositing imidazole type ion liquid and phosphomolybdic acid again, makes to be superimposed in the form of stratiform between each component, be conducive to photoelectronic
Rule transmitting, stablizes electrode performance.
The present invention also provides the preparation methods of the Combined electrode, at least include the following steps,
(1) using the matrix of at least surface titaniferous as anode, pass through anodizing in-situ preparation dioxy on the matrix
Change titanium nanotube；
(2) the acidification carbon nanotube is carried on the titania nanotube through cyclic voltammetry and obtains compound load
Body；
(3) successively imidazole type ion liquid and phosphomolybdic acid are deposited on the complex carrier by infusion process.
Preparation method step of the invention is simple, mild condition, and not needing special installation can be prepared by the combination electrode, tool
There is the prospect of industrial applications.
Preferably, the matrix of at least surface titaniferous is the substrate that pure titanium-based material or surface are coated with titanium film.
Preferably, in step (1), the anodizing are as follows: in the reaction that the anode and cathode and electrolyte form
Under system, energization aoxidizes the anode, then calcines；The cathode is platinum electrode, and the electrolyte is by fluoride ion
Compound, rudimentary saturated alcohols and deionized water composition.
It is further preferred that the distance between anode and cathode is 1~2cm in the anodizing, the energization is
Logical 40~60V direct current, 2~3h of conduction time.
It is further preferred that the calcining is to calcine 3~4h at 400~500 DEG C.
It is further preferred that in the electrolyte fluoride ion compound concentration be 0.1~0.2mol/L, it is described go from
The volumetric concentration of sub- water is 3~5%, and fluoride ion compound is optional but is not limited to ammonium fluoride, and saturation lower alcohol is optional but unlimited
In ethylene glycol.
Preferred anodic oxidation condition can form the good titania nanotube of uniform form in matrix surface.
Preferably, in step (2), the cyclic voltammetry are as follows: have nano titania with surface array obtained by step (1)
The matrix of pipe is anode, and using platinum electrode as cathode, calomel electrode is reference electrode, constitutes three-electrode system, with containing 0.4~
The solution that 0.6mg/mL is acidified carbon nanotube is electrolyte, and scanning range -1.5V~0.5V sweeps 50~60mv/s of speed, scanning 20
~30 circles.
Preferred cyclic voltammetry condition can be such that acidification carbon nanotube is uniformly carried on titania nanotube securely.
Be acidified carbon nanotube the optional this field of preparation method conventional method, such as: by carbon nanotube in concentrated hydrochloric acid ultrasonic disperse, clearly
It washes after drying and aoxidizes 8h at 70 DEG C with the concentrated sulfuric acid of volume ratio 3:1 and concentrated nitric acid, be drying to obtain after being cleaned with ultrapure water.
Preferably, in step (3), the method that loads imidazole type ion liquid are as follows: will be impregnated after complex carrier activation
20~30min in 4~6wt% ionic liquid solution；The method for loading phosphomolybdic acid are as follows: load is had into imidazole type ion liquid
Complex carrier is impregnated in 20~30min in the phosphorus molybdenum acid solution of 4~6mmol/L.
The activation method of the complex carrier is optionally: being dipped in 2~4min in the nitric acid of 9~10mol/L.
The present invention is by infusion process supported ion liquid and phosphomolybdic acid on complex carrier, and method is easy, and ionic liquid
It is connected in a manner of layer self assembly with phosphomolybdic acid, is conducive to photoelectronic rule transmitting and conversion.
The present invention also provides application of the Combined electrode in photoelectric catalysis degrading polycyclic aromatic hydrocarbon, in visible light or
Under ultraviolet irradiation condition, lower current density can the polycyclic aromatic hydrocarbons such as efficient degradation phenanthrene.
Detailed description of the invention
Fig. 1 is the forming process schematic diagram of combination electrode of the present invention, wherein CNTs be carbon nanotube, RTIL be imidazole type from
Sub- liquid, POM are phosphomolybdic acid.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, with reference to embodiments, to the present invention
It is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, it is not used to
Limit the present invention.
Embodiment 1
The combination electrode of the present embodiment successively includes matrix titanium foil, titania nanotube, acidification carbon nanometer from the inside to the outside
Pipe, 1- butyl -3- methylimidazolium hydrogen sulphate salt and phosphomolybdic acid.
The combination electrode the preparation method is as follows:
1, substrate pretreated
The sand paper of 500 mesh of titanium foil is polished to remove titanium foil surface impurity；By the titanium foil after polishing be respectively placed in acetone,
In ethyl alcohol, isopropanol and ultrasound, the titanium foil after cleaning ultrasound with deionized water spontaneously dry at room temperature.
2, titania nanotube is prepared
(1) electrolyte quota: using the solution that ethylene glycol, deionized water and ammonium fluoride form as electrolyte, wherein ammonium fluoride
Concentration be 0.15mol/L, the volume fraction of deionized water is 4%.
(2) anodic oxidation: as anode, platinum plate electrode being cathode using the titanium foil that step 1 is handled, between anode and cathode away from
From for 2cm, 50V DC voltage 2h is led in above-mentioned electrolyte, carries out anodic oxidation；Titanium is cleaned with deionized water after oxidation
Foil calcines 3h at 450 DEG C, spare after cooling；
3, deposition acidification carbon nanotube
(1) it is acidified the preparation of carbon nanotube: ultrasonic disperse in concentrated hydrochloric acid is added in carbon nanotube, is stood overnight, is filtered, is surpassed
It is dry after pure water.The carbon nanotube of above-mentioned processing is added in the concentrated sulfuric acid and concentrated nitric acid mixed liquor of volume ratio 3:1,70 DEG C
Water-bath aoxidizes 8h, filters, dry after milli-Q water.
(2) above-mentioned acidification carbon nanotube cyclic voltammetry deposition acidification carbon nanotube: is added to the phosphoric acid hydrogen of 0.1mol/L
In two sodium solutions, concentration 0.5mg/mL；There is the titanium foil of titania nanotube as anode, platinum filament using surface prepared by step 2
Electrode is cathode, and calomel electrode is reference electrode, constitutes three-electrode system, and scanning range -1.5V~0.5V sweeps fast 50mv/s,
20 circle of scanning；Acidification carbon nanotube in above-mentioned disodium phosphate soln is deposited on titanium foil, after it is clear with deionized water
Titanium foil is washed, is dried at room temperature, it is spare.
4, imidazole ion liquid is loaded
Titanium foil of the step 3 after dry is dipped in 2min in the nitric acid of 9mol/L, to activate the carbon nanotube of load, after taking-up
It is cleaned with deionized water, is then dipped in 20min in 5wt% imidazole ion liquid deionized water solution, is cleaned with deionized water.
5, phosphomolybdic acid is loaded
Titanium foil after step 4 cleaning is dipped in 20min in the phosphomolybdic acid deionized water solution of 5mmol/L, uses deionized water
Cleaning is dried at room temperature to get Combined electrode.
Embodiment 2
The combination electrode of the present embodiment successively includes matrix titanium foil, titania nanotube, acidification carbon nanometer from the inside to the outside
Pipe, 1- butyl -3- methylimidazolium chloride and phosphomolybdic acid.
The combination electrode the preparation method is as follows:
1, substrate pretreated
The sand paper of 500 mesh of titanium foil is polished to remove titanium foil surface impurity；By the titanium foil after polishing be respectively placed in acetone,
In ethyl alcohol, isopropanol and ultrasound, the titanium foil after cleaning ultrasound with deionized water spontaneously dry at room temperature.
2, titania nanotube is prepared
(1) electrolyte quota: using the solution that ethylene glycol, deionized water and ammonium fluoride form as electrolyte, wherein ammonium fluoride
Concentration be 0.1mol/L, the volume fraction of deionized water is 5%.
(2) anodic oxidation: as anode, platinum plate electrode being cathode using the titanium foil that step 1 is handled, between anode and cathode away from
From for 1cm, 40V DC voltage 3h is led in above-mentioned electrolyte, carries out anodic oxidation；Titanium is cleaned with deionized water after oxidation
Foil calcines 4h at 400 DEG C, spare after cooling；
3, deposition acidification carbon nanotube
(1) it is acidified the preparation of carbon nanotube: ultrasonic disperse in concentrated hydrochloric acid is added in carbon nanotube, is stood overnight, is filtered, is surpassed
It is dry after pure water.The carbon nanotube of above-mentioned processing is added in the concentrated sulfuric acid and concentrated nitric acid mixed liquor of volume ratio 3:1,70 DEG C
Water-bath aoxidizes 8h, filters, dry after milli-Q water.
(2) above-mentioned acidification carbon nanotube cyclic voltammetry deposition acidification carbon nanotube: is added to the phosphoric acid hydrogen of 0.1mol/L
In two sodium solutions, concentration 0.4mg/mL；There is the titanium foil of titania nanotube as anode, platinum filament using surface prepared by step 2
Electrode is cathode, and calomel electrode is reference electrode, constitutes three-electrode system, and scanning range -1.5V~0.5V sweeps fast 60mv/s,
20 circle of scanning；Acidification carbon nanotube in above-mentioned disodium phosphate soln is deposited on titanium foil, after it is clear with deionized water
Titanium foil is washed, is dried at room temperature, it is spare.
4, imidazole ion liquid is loaded
Titanium foil of the step 3 after dry is dipped in 2min in the nitric acid of 9mol/L, to activate the carbon nanotube of load, after taking-up
It is cleaned with deionized water, is then dipped in 30min in 4wt% imidazole ion liquid aqueous solution, is cleaned with deionized water.
5, phosphomolybdic acid is loaded
Titanium foil after step 4 cleaning is dipped in 20min in the phosphomolybdic acid aqueous solution of 6mmol/L, is cleaned with deionized water, room
Temperature is lower dry to get Combined electrode.
Embodiment 3
The combination electrode of the present embodiment successively includes matrix titanium foil, titania nanotube, acidification carbon nanometer from the inside to the outside
Pipe, 1- butyl -3- methylimidazolium hydrogen sulphate salt and phosphomolybdic acid.
The combination electrode the preparation method is as follows:
1, substrate pretreated
The sand paper of 500 mesh of titanium foil is polished to remove titanium foil surface impurity；By the titanium foil after polishing be respectively placed in acetone,
In ethyl alcohol, isopropanol and ultrasound, the titanium foil after cleaning ultrasound with deionized water spontaneously dry at room temperature.
2, titania nanotube is prepared
(1) electrolyte quota: using the solution that ethylene glycol, deionized water and ammonium fluoride form as electrolyte, wherein ammonium fluoride
Concentration be 0.2mol/L, the volume fraction of deionized water is 3%.
(2) anodic oxidation: as anode, platinum plate electrode being cathode using the titanium foil that step 1 is handled, between anode and cathode away from
From for 2cm, 60V DC voltage 2h is led in above-mentioned electrolyte, carries out anodic oxidation；Titanium is cleaned with deionized water after oxidation
Foil calcines 3h at 500 DEG C, spare after cooling；
3, deposition acidification carbon nanotube
(1) it is acidified the preparation of carbon nanotube: ultrasonic disperse in concentrated hydrochloric acid is added in carbon nanotube, is stood overnight, is filtered, is surpassed
It is dry after pure water.The carbon nanotube of above-mentioned processing is added in the concentrated sulfuric acid and concentrated nitric acid mixed liquor of volume ratio 3:1,70 DEG C
Water-bath aoxidizes 8h, filters, dry after milli-Q water.
(2) above-mentioned acidification carbon nanotube cyclic voltammetry deposition acidification carbon nanotube: is added to the phosphoric acid hydrogen of 0.1mol/L
In two sodium solutions, concentration 0.5mg/mL；There is the titanium foil of titania nanotube as anode, platinum filament using surface prepared by step 2
Electrode is cathode, and calomel electrode is reference electrode, constitutes three-electrode system, and scanning range -1.5V~0.5V sweeps fast 50mv/s,
30 circle of scanning；Acidification carbon nanotube in above-mentioned disodium phosphate soln is deposited on titanium foil, after it is clear with deionized water
Titanium foil is washed, is dried at room temperature, it is spare.
4, imidazole ion liquid is loaded
Titanium foil of the step 3 after dry is dipped in 2min in the nitric acid of 9mol/L, to activate the carbon nanotube of load, after taking-up
It is cleaned with deionized water, is then dipped in 20min in 6wt% imidazole ion liquid aqueous solution, is cleaned with deionized water.
5, phosphomolybdic acid is loaded
Titanium foil after step 4 cleaning is dipped in 30min in the phosphomolybdic acid aqueous solution of 4mmol/L, is cleaned with deionized water, room
Temperature is lower dry to get Combined electrode.
Technical solution in order to better illustrate the present invention is done by comparative example and the embodiment of the present invention into one further below
The comparison of step.
Comparative example 1
The combination electrode is that the complex carrier prepared according to the method for 1 step 1~3 of embodiment (includes matrix, titanium dioxide
Titanium nanotube and carbon nanotube).
Comparative example 2
Complex carrier is prepared according to the method for 1 step 1~3 of embodiment, is made with tetrabutylammonium bromide and phosphomolybdic acid reaction
(NBu4)3PMo12O40, complex carrier is dipped in (the NBu of 5mg/mL4)3PMo12O40In acetonitrile solution, combination electrode is made.
Effect example 1
The combination electrode of Examples 1 to 3 and comparative example 1~2 is used for photoelectric catalysis degrading phenanthrene respectively, experimental procedure is such as
Under: be cathode using the combination electrode as anode, platinum plate electrode, calomel electrode in the three-electrode system of reference electrode to containing
The waste water of 1.5mg/L phenanthrene carries out Degrading experiment, and it is 50 μ A/cm that constant current is kept using xenon lamp as light source, in degradation process2, degradation
Time is 1h.Degradation results are as shown in table 1.
The test of 1 embodiment and comparative example electrode degrading phenanthrene of table
Effect example 2
The combination electrode of Examples 1 to 3 is recycled and reused for photoelectrochemical degradation phenanthrene, still has 90% or more after reusing 6 times
Degradation rate.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention
Made any modification, equivalent replacement or improvement etc., should all be included in the protection scope of the present invention within mind and principle.
Claims (10)
1. a kind of Combined electrode, which is characterized in that its successively include: from the inside to the outside electrode matrix, titania nanotube,
It is acidified carbon nanotube, imidazole type ion liquid and phosphomolybdic acid.
2. Combined electrode as described in claim 1, which is characterized in that it is that titanium dioxide is made on electrode matrix to receive
Mitron, then will be acidified it is carbon nanotube loaded on the titania nanotube, be then sequentially depositing imidazole type ion liquid and
The Combined electrode is made in phosphomolybdic acid.
3. the preparation method of Combined electrode as claimed in claim 1 or 2, which is characterized in that it at least includes the following steps,
(1) using the matrix of at least surface titaniferous as anode, pass through anodizing in-situ preparation titanium dioxide on the matrix
Nanotube；
(2) the acidification carbon nanotube is carried on the titania nanotube through cyclic voltammetry and obtains complex carrier；
(3) successively imidazole type ion liquid and phosphomolybdic acid are deposited on the complex carrier by infusion process.
4. preparation method as claimed in claim 3, which is characterized in that the matrix of at least surface titaniferous be pure titanium-based material or
Surface is coated with the substrate of titanium film.
5. preparation method as claimed in claim 3, which is characterized in that in step (1), the anodizing are as follows: described
Under anode and cathode and the reaction system of electrolyte composition, energization aoxidizes the anode, then calcines；The cathode is
Platinum electrode, the electrolyte are made of fluoride ion compound, rudimentary saturated alcohols and deionized water.
6. preparation method as claimed in claim 5, which is characterized in that in the anodizing, between anode and cathode
Distance is 1~2cm, described to be powered as logical 40~60V direct current, 2~3h of conduction time；And/or:
The calcining is that 3~4h is calcined at 400~500 DEG C；And/or:
The concentration of fluoride ion compound is 0.1~0.2mol/L in the electrolyte, and the volumetric concentration of the deionized water is 3
~5%.
7. preparation method as claimed in claim 3, which is characterized in that in step (2), the cyclic voltammetry are as follows: with step
(1) it is anode that gained surface array, which has the matrix of titania nanotube, and using platinum electrode as cathode, calomel electrode is reference electricity
Pole constitutes three-electrode system, using the solution containing 0.4~0.6mg/mL acidification carbon nanotube as electrolyte, scanning range -1.5V
~0.5V sweeps 50~60mv/s of speed, 20~30 circle of scanning.
8. preparation method as claimed in claim 3, which is characterized in that in step (3), the method that loads imidazole type ion liquid
Are as follows: 20~30min in 4~6wt% ionic liquid solution will be impregnated in after complex carrier activation；And/or:
The method for loading phosphomolybdic acid are as follows: the complex carrier that load has imidazole type ion liquid is impregnated in the phosphorus molybdenum of 4~6mmol/L
20~30min in acid solution.
9. preparation method as claimed in claim 8, which is characterized in that the activation method of the complex carrier are as follows: be dipped in 9
2~4min in the nitric acid of~10mol/L.
10. application of the Combined electrode of any of claims 1 or 2 in photoelectric catalysis degrading polycyclic aromatic hydrocarbon.
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