CN110272100A - Ti4O7Preparation method of ceramic microfiltration membrane electrode of coating - Google Patents
Ti4O7Preparation method of ceramic microfiltration membrane electrode of coating Download PDFInfo
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- CN110272100A CN110272100A CN201910477152.3A CN201910477152A CN110272100A CN 110272100 A CN110272100 A CN 110272100A CN 201910477152 A CN201910477152 A CN 201910477152A CN 110272100 A CN110272100 A CN 110272100A
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- 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
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- 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
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- 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
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- 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
- C02F2001/46152—Electrodes characterised by the shape or form
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- 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
Abstract
The invention relates to Ti4O7The preparation method of the ceramic micro-filtration membrane electrode comprises the steps of preparing a polyvinyl alcohol solution from ⑴, adding titanium dioxide, polyacrylic acid, glycerol and polyvinylpyrrolidone, and forming Ti by mechanical stirring4O7Precursor sol ⑵ immersing flat ceramic micro-filter membrane in Ti obtained in step ⑴4O7Dipping the precursor sol into the surface of a flat ceramic microfiltration membrane by lifting and coating Ti4O7Drying the precursor sol film in air to form Ti4O7Precursor gel coated ceramic microfilter membrane electrode ⑶ Ti is obtained from ⑵4O7Putting the precursor gel coated ceramic microfiltration membrane electrode in a muffle furnace for annealing, and cooling to form Ti4O7⑷ Ti synthesized in step ⑶4O7Annealing and reducing the ceramic microfiltration membrane electrode of the precursor coating in the atmosphere of hydrogen to finally form Ti4O7The ceramic microfiltration membrane electrode of the coating.
Description
Technical field
The present invention relates to electrocatalysis high-grade oxidized field, in particular to a kind of oxidative degradation of organic wastewater with difficult degradation thereby
Ti4O7The preparation method of the ceramic micro filter membrane electrode of coating.
Background technique
With the rapid development of China's industry, urban population is constantly expanded, and is produced during economical production and daily life
A large amount of organic wastewater with difficult degradation thereby is given birth to.Organic wastewater with difficult degradation thereby usually has the spies such as biodegradability is low, water quality is complicated, toxicity is high
Point can not be eradicated thoroughly with traditional processing method.In recent years, in large- and-medium size cities organic wastewater with difficult degradation thereby annual output be in by
Year ascendant trend solves the problems, such as that countermeasure is to perplex various regions government.High-level oxidation technology is fast with reaction speed, technique is opposite
Simply, the advantages that high treating effect, there is good prospect in terms of the advanced treating of organic wastewater with difficult degradation thereby.Electrocatalytic oxidation
It is one kind of high-level oxidation technology, hydroxyl radical free radical or oxidant is directly or indirectly generated to organic matter by electro-catalysis process
Carry out oxidative degradation.Electro-catalytic oxidation technology is with easy to operate, organic matter degradation mineralising is high-efficient, service condition is mild, produces
Many advantages, such as raw secondary pollution is few, reaction controllability is strong, it is considered to be most the organic wastewater with difficult degradation thereby of prospect handles skill
Art.
Electrode material is the core of electrocatalytic oxidation.The anode generallyd use in electrocatalytic oxidation technique in recent years mainly wraps
Include metal oxide electrode, dimensional stability (DSA) electrode and boron-doped diamond (BDD) electrode.Metal oxide electrode have compared with
The advantages that wide electrochemical window, high stability, low cost.Research has shown that, in SnO2And PbO2Electrode surface can produce hydroxyl certainly
By base.However simple SnO2And PbO2Electric conductivity it is poor, need to be doped improve metal oxide electric conductivity, but
The service life of electrode can be greatly shortened after doping.In addition, Sn and Pb has toxicity, certain Pb can be generated in electrolytic process2+
And Sn2+Ion penetrates into waste water, causes the secondary pollution of water body.DSA electrode is the Ti base electrode of catalyst coat, due to
Ti has strong electric conductivity and stability, is better than in corrosion resistance and in terms of electrode life metal oxide and graphite electrode, this
The cost of outer Ti is far below rare metal Pt, therefore DSA electrode has a good application prospect.DSA electrode is aoxidized compared to metal
Object electrode overcomes the disadvantages of metal autolysis is polluted caused by electrolyte, but shape is easy between DSA electrode Ti and plated film
At passivation layer, it is suppressed that the electrical conductive activities of electrode, and under the conditions of corrosive solution is with there is gas evolution, Catalytic Layer is easily broken
And damage, influence electrode life.BDD electrode is the anode of best performance in current electrocatalytic oxidation system, by diamond
Boron is adulterated in crystal, makes it have certain electric conductivity.Since carbon atom is hybridized to SP in BDD electrode3Hydridization, electron cloud knot
Structure is more stable, makes it have higher oxygen evolution potential.In addition, BDD electrode also has strong corrosion resistance and good chemistry steady
It is qualitative, and there is very strong physisorption to hydroxyl radical free radical, therefore have to organic pollutant oxidative degradation mineralising
Higher reactivity.But BDD electrode still has limitation, existing multidigit researcher observes in BDD electrode surface meeting
Polymer film is formed to which the passivation phenomenon of electrode occur, eventually leads to the decline of electrochemicial oxidation efficiency, electrode uses
Service life reduction.The internal resistance with higher of BDD electrode causes it to generate heat in electrolytic process seriously, reduces current efficiency and contracting
Short service life.Furthermore the high cost of BDD electrode limits its large-scale application in practical projects.In recent years, sub-
Titanium oxide electrode is considered current due to the cost of its high conductivity, strong corrosion resistant, high oxygen evolution potential and relative moderate
The most promising anode material in electrocatalytic oxidation system.Sub- titania meterial is to a series of non-stoichiometric formulas
The general designation of titanium oxide, general formula TinO2n-1(4≤n≤10).In all sub- titania meterials, the sub- oxygen of Magn é li phase
Change titanium Ti4O7Electric conductivity highest (1500s/cm), be three times of graphite, and Ebonex is registered as by offshore company@Quotient
Mark.Ti4O7Structure be based on rutile TiO2, every 4 layers of rutile structure unit, there is a shared oxygen atom shear surface.
Ti4O7Compared to Titanium there is outstanding corrosion resistant to light up performance, under room temperature, not with sulfuric acid, nitric acid, hydrochloric acid and caustic soda reaction.In addition,
Ti4O7Electrochemical properties it is highly stable, oxygen evolution potential proves have to organic wastewater with difficult degradation thereby up to 2.5Vvs.SHE
Good electrolytic catalysis effect.
Summary of the invention
Technical problem solved by the invention is to overcome in current electrocatalytic oxidation technique that electrode is at high cost, effect is poor not
It provides enough a kind of by control Ti4O7Annealing temperature and annealing of the ceramic micro filter membrane electrode of coating in annealing reduction process
Time, to produce pure phase Ti4O7The ceramic micro filter membrane electrode of coating.Another technical problem solved by the invention is to provide
A kind of method is simple, at low cost, electrolysis effectiveness is stable, current potential window width, use high-efficient to the electrolytic catalysis of hardly degraded organic substance
The Ti of service life length4O7The preparation method of the ceramic micro filter membrane electrode of coating.
The technical solution of the invention is as follows the Ti4O7The preparation method of coating ceramic micro-filtration membrane electrode, special character
It is, comprising the following steps:
(1) polyvinyl alcohol (PVA) solution is configured, and adds titanium dioxide (TiO according to this2), polyacrylic acid (PAA), glycerol and
Polyvinylpyrrolidone (PVP) then forms Ti by mechanical stirring4O7Precursor sol;
(2) flat ceramic microfiltration membranes are immersed to the Ti (1) obtained by step4O7In precursor sol, it is immersed in by lifting flat
Plate ceramic micro filter film surface coats one layer of Ti4O7Precursor sol film is subsequently placed at air drying and forms Ti4O7Presoma is solidifying
The ceramic micro filter membrane electrode of glue coating;
(3) the Ti (2) step obtained4O7The ceramic micro filter membrane electrode of aqueous precursor gel coating, which is placed in Muffle furnace, to be moved back
Igneous type forms Ti after cooling4O7The ceramic micro filter membrane electrode of presoma coating;
(4) the Ti (3) step synthesized4O7The ceramic micro filter membrane electrode of presoma coating is annealed in the atmosphere of hydrogen
Reduction, ultimately forms Ti4O7The ceramic micro filter membrane electrode of coating.
As preferred: the step (1) titanium dioxide (TiO2) average grain diameter be 0.5~2 μm.
As preferred: the step (1) Ti4O7The concentration of PVA is 30~200mg/L, TiO in precursor sol solution2
Concentration be 100~200mg/L, the concentration of PAA is 1~3mg/L, and the concentration of glycerol is 1~2mg/L, the concentration of PVP is 1~
1.5mg/L。
As preferred: to improve Ti4O7The viscosity of precursor sol and the stability of film forming, the PVA concentration in the colloidal sol
For 100mg/L;To improve Ti4O7The stability and Ti of presoma coating4O7Presoma content, the TiO in the colloidal sol2Concentration is
200mg/L。
As preferred: PAA concentration of the step (1) in the colloidal sol is 1~3mg/L, and glycerol concentration is 1~2mg/L, PVP
Concentration is 1.5mg/L.
As preferred: (2) the flat ceramic microfiltration membranes immerse Ti to step4O7The time of precursor sol is 16~36s,
The rate of pulling is 5~20cm/s.
As preferred: the step (4) Ti4O7Annealing temperature needed for the ceramic micro filter film electrode moulding of presoma coating
It is 800~1000 DEG C, annealing time is 2~4h.
As preferred: the step (4) Ti4O7The ceramic micro filter membrane electrode of presoma coating is in annealing reduction process
Annealing temperature is 900~1050 DEG C, and annealing time is 2~4h, and the flow of hydrogen is 40~120ml/min.
As preferred: the step (4) Ti4O7Aqueous precursor gel coating ceramic micro filter film annealing temperature be 800~
1000 DEG C, annealing time is 2~4h.
Compared with prior art, beneficial effects of the present invention:
(1) Ti of the present invention4O7Coated crystal composition, oxygen evolution potential measurement and the configuration of surface of the ceramic micro filter membrane electrode of coating
Analysis:
The Ti of pure phase obtained is tested using X-ray diffractometer (Ultima IV, Rigaku Co.Ltd., Japan)4O7It applies
The crystal composition of the ceramic micro filter film electrode coating of layer, it is found that the crystal group of the coating of electrode becomes the Ti of pure phase4O7;Using electricity
Chem workstation (CHI760D, Chenhua Instrument Co.Ltd., Shanghai, China) tests Ti4O7The pottery of coating
Porcelain microfiltration membranes polarization of electrode curve, and then determine the oxygen evolution potential of electrode, scanning range is 1~3V vs.SHE, sweep speed
For 5mV/s, Ti is found4O7The oxygen evolution potential of the ceramic micro filter membrane electrode of coating is up to 2.20Vvs.SHE, higher than Pt electrode
1.84Vvs.SHE;Ti is analyzed using scanning electron microscope (Mira3, Tescan, Czech Republic)4O7The ceramic micro filter film of coating
The configuration of surface of electrode finds Ti4O7Particle partial melting forms reticular structure, and generates a large amount of hole, the aperture collection of hole
In be distributed in 1~2 μ m.
(2) Ti of the present invention4O7The ceramic micro filter membrane electrode of coating is in electrocatalysis high-grade oxidized process to hardly degraded organic substance
Function and effect analysis:
Respectively with Pt electrode and Ti4O7The ceramic micro filter membrane electrode of coating carries out Electro-catalytic Oxidation Process azo as anode
The experiment of dyestuff orange beta-naphthol water distribution is tested in homeostasis current density (20mA/cm2) under conditions of carry out, pass through ultraviolet spectrometry light
The concentration of orange beta-naphthol in degree meter (UV-2450, Shimadzu, Kyoto, Japan) measurement water distribution.Experiment discovery, with Ti4O7Coating
Ceramic micro filter membrane electrode can will be orange in solution in the degradation process of 1h as the electrocatalytic oxidation system of anode
II concentration from 21.51mg/L be reduced to 1mg/L hereinafter, and using Pt electrode as the electrocatalytic oxidation system of anode 2.5h degradation
In the process, the orange beta-naphthol concentration in solution is only capable of being reduced to 13.368mg/L from 21.51mg/L.Research has shown that Ti4O7The pottery of coating
Porcelain micro-filtration membrane electrode has extremely strong Electrocatalysis Degradation effect to hardly degraded organic substance.
(3) Ti of the present invention4O7Annealing temperature and annealing time of the ceramic micro filter membrane electrode of coating in annealing reduction process
To produce pure phase Ti4O7The ceramic micro filter membrane electrode of coating.The production method of electrode of the present invention is simple, at low cost, electrolysis is imitated
Fruit stabilization, current potential window width, long service life high-efficient to the electrolytic catalysis of hardly degraded organic substance.
(4) the present invention improves Ti4O7The viscosity of precursor sol and the stability of film forming and Ti4O7Presoma coating it is steady
Qualitative and Ti4O7Presoma content reduces Ti4O7The moisture content of aqueous precursor gel film and inhibition are cracked during annealing molding
Generation rate.
Detailed description of the invention
Fig. 1 is Ti of the present invention4O7Precursor sol pictorial diagram;
Fig. 2 is Ti of the present invention4O7The ceramic micro filter membrane electrode pictorial diagram of coating;
Fig. 3 is Ti of the present invention4O7The X ray diffracting spectrum of the ceramic micro filter membrane electrode of coating;
Fig. 4 is Ti of the present invention4O7The ceramic micro filter membrane electrode and Pt polarization of electrode curve graph of coating;
Fig. 5 is Ti of the present invention4O7The scanning electron microscope imaging figure of the ceramic micro filter membrane electrode of coating;
Fig. 6 is Ti4O7The effect of the electrocatalysis high-grade oxidized degradation orange beta-naphthol water distribution of the ceramic micro filter membrane electrode and Pt electrode of coating
Fruit figure.
Specific embodiment
The present invention will now be further detailed embodiment:
Ti4O7The preparation method of the ceramic micro filter membrane electrode of coating, comprising the following steps:
⑴Ti4O7The preparation of precursor sol:
Take 10gPVA to be placed in a beaker, pour into deionized water to 100ml, after place the beaker 105 DEG C heating plate (IKA,
RT-10 so that PVA dissolves on), deionized water is added in right amount to supplement the evaporation loss of deionized water in course of dissolution;After cooling
20gTiO is added according to this2, 2gPAA, 1.5g glycerol and 1.2gPVP and stir, be finally settled to 100ml with deionized water;With stirring
It mixes device (IKA, RW-20) and mechanical stirring is carried out to colloidal sol to enhance TiO with 900rpm revolving speed2Dispersibility in colloidal sol, stirring
Ti is obtained afterwards4O7Precursor sol;
⑵Ti4O7The preparation of the ceramic micro filter film of aqueous precursor gel coating:
Ti is carried out using PTL-OV5P pulling coating machine4O7The preparation of the ceramic micro filter film of aqueous precursor gel coating, will be ultrasonic
Flat ceramic microfiltration membranes (25mm × 30mm, 1 μm of average pore size) after cleaning are fixed on lifting platform, after by flat ceramic micro-filtration
Film immerses Ti4O7In precursor sol, dip time continues 25s, with the speed of 10cm/s by flat ceramic micro-filtration after the completion of dipping
Film at the uniform velocity lifts rising, with Ti4O7Precursor sol separation, after spontaneously dried under conditions of 25 DEG C and relative humidity are 30%
18h forms Ti4O7The ceramic micro filter film of aqueous precursor gel coating;
⑶Ti4O7The annealing of the ceramic micro filter film of presoma coating forms:
By the Ti after drying4O7The ceramic micro filter film of aqueous precursor gel coating is placed in Muffle furnace (KSL-1200X-J),
Be warming up to 1000 DEG C, constant temperature 4h with the speed of 5 DEG C/min, after be cooled to room temperature after obtain Ti4O7The ceramics of presoma coating are micro-
Filter membrane;
⑷Ti4O7The annealing of the ceramic micro filter membrane electrode of coating restores:
It will obtain Ti4O7The ceramic micro filter film of presoma coating is placed in tube furnace (OTF-1200X-II), with hydrogen
(80mL/min) be used as carrier gas, be warming up to 950 DEG C, constant temperature 2h with the speed of 5 DEG C/min, after be cooled to room temperature after obtain Ti4O7
The ceramic micro filter membrane electrode of coating;
⑸Ti4O7Coated crystal composition, oxygen evolution potential measurement and the configuration of surface analysis of the ceramic micro filter membrane electrode of coating:
The Ti of pure phase obtained is tested using X-ray diffractometer (UltimaIV, Rigaku Co.Ltd.Japan)4O7Coating
Ceramic micro filter film electrode coating crystal composition, find the coating of electrode crystal group become pure phase Ti4O7;Using electrification
It learns work station (CHI760D, Chenhua Instrument Co.Ltd., Shanghai, China) and tests Ti4O7The ceramics of coating
Microfiltration membranes polarization of electrode curve, and then determine the oxygen evolution potential of electrode, scanning range is 1~3Vvs.SHE, and sweep speed is
5mV/s has found Ti4O7The oxygen evolution potential of the ceramic micro filter membrane electrode of coating is up to 2.20Vvs.SHE, higher than Pt electrode
1.84Vvs.SHE;Ti is analyzed using scanning electron microscope (Mira3, Tescan, Czech Republic)4O7The ceramic micro filter film of coating
The configuration of surface of electrode finds Ti4O7Particle partial melting forms reticular structure, and generates a large amount of hole, the aperture collection of hole
In be distributed in 1~2 μ m;
⑸Ti4O7The ceramic micro filter membrane electrode of coating imitates the effect of hardly degraded organic substance in electrocatalysis high-grade oxidized process
Fruit analysis:
Respectively with Pt electrode and Ti4O7The ceramic micro filter membrane electrode of coating carries out Electro-catalytic Oxidation Process azo as anode
The experiment of dyestuff orange beta-naphthol water distribution is tested in homeostasis current density (20mA/cm2) under conditions of carry out, pass through ultraviolet spectrometry light
The concentration of orange beta-naphthol in degree meter (UV-2450, Shimadzu, Kyoto, Japan) measurement water distribution.Experiment discovery, with Ti4O7Coating
Ceramic micro filter membrane electrode can will be orange in solution in the degradation process of 1h as the electrocatalytic oxidation system of anode
II concentration from 21.51mg/L be reduced to 1mg/L hereinafter, and using Pt electrode as the electrocatalytic oxidation system of anode 2.5h degradation
In the process, the orange beta-naphthol concentration in solution is only capable of being reduced to 13.368mg/L from 21.51mg/L.Research has shown that Ti4O7The pottery of coating
Porcelain micro-filtration membrane electrode has extremely strong Electrocatalysis Degradation effect to hardly degraded organic substance.
The foregoing is merely presently preferred embodiments of the present invention, all equivalent changes done according to scope of the invention as claimed with
Modification, should all belong to the covering scope of the claims in the present invention.
Claims (9)
1. a kind of Ti4O7The preparation method of coating ceramic micro-filtration membrane electrode, which comprises the following steps:
(1) polyvinyl alcohol (PVA) solution is configured, and adds titanium dioxide (TiO according to this2), polyacrylic acid (PAA), glycerol and poly- second
Alkene pyrrolidone (PVP) then forms Ti by mechanical stirring4O7Precursor sol;
(2) flat ceramic microfiltration membranes are immersed to the Ti (1) obtained by step4O7In precursor sol, plate pottery is immersed in by lifting
Porcelain micro-filtration film surface coats one layer of Ti4O7Precursor sol film is subsequently placed at air drying and forms Ti4O7Aqueous precursor gel applies
The ceramic micro filter membrane electrode covered;
(3) the Ti (2) step obtained4O7The ceramic micro filter membrane electrode of aqueous precursor gel coating, which is placed in Muffle furnace, to be annealed into
Type forms Ti after cooling4O7The ceramic micro filter membrane electrode of presoma coating;
(4) the Ti (3) step synthesized4O7The ceramic micro filter membrane electrode of presoma coating carries out annealing reduction in the atmosphere of hydrogen,
Ultimately form Ti4O7The ceramic micro filter membrane electrode of coating.
2. Ti according to claim 14O7The preparation method of the ceramic micro filter membrane electrode of coating, which is characterized in that step (1) institute
Titanium dioxide (the TiO stated2) average grain diameter be 0.5~2 μm.
3. Ti according to claim 14O7The preparation method of the ceramic micro filter membrane electrode of coating, which is characterized in that step (1) institute
The Ti stated4O7The concentration of PVA is 30~200mg/L, TiO in precursor sol solution2Concentration be 100~200mg/L, PAA's
Concentration is 1~3mg/L, and the concentration of glycerol is 1~2mg/L, and the concentration of PVP is 1~1.5mg/L.
4. Ti according to claim 34O7The preparation method of the ceramic micro filter membrane electrode of coating, which is characterized in that improve
Ti4O7The viscosity of precursor sol and the stability of film forming, the PVA concentration in the colloidal sol are 100mg/L;To improve Ti4O7Before
Drive the stability and Ti of body coating4O7Presoma content, the TiO in the colloidal sol2Concentration is 200mg/L.
5. Ti according to claim 14O7The preparation method of the ceramic micro filter membrane electrode of coating, which is characterized in that step (1) institute
PAA concentration in the colloidal sol stated is 1~3mg/L, and glycerol concentration is 1~2mg/L, and PVP concentration is 1.5mg/L.
6. Ti according to claim 14O7The preparation method of the ceramic micro filter membrane electrode of coating, which is characterized in that step (2) institute
The flat ceramic microfiltration membranes stated immerse Ti4O7The time of precursor sol is 16~36s, and the rate of pulling is 5~20cm/s.
7. Ti according to claim 14O7The preparation method of the ceramic micro filter membrane electrode of coating, which is characterized in that step (4) institute
The Ti stated4O7Annealing temperature needed for the ceramic micro filter film electrode moulding of presoma coating is 800~1000 DEG C, annealing time 2
~4h.
8. Ti according to claim 14O7The preparation method of the ceramic micro filter membrane electrode of coating, which is characterized in that step (4) institute
The Ti stated4O7Annealing temperature of the ceramic micro filter membrane electrode of presoma coating in annealing reduction process is 900~1050 DEG C, is moved back
The fiery time is 2~4h, and the flow of hydrogen is 40~120ml/min.
9. Ti according to claim 14O7The preparation method of the ceramic micro filter membrane electrode of coating, which is characterized in that step (4) institute
State Ti4O7The annealing temperature of the ceramic micro filter film of aqueous precursor gel coating is 800~1000 DEG C, and annealing time is 2~4h.
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CN111592078A (en) * | 2020-05-09 | 2020-08-28 | 哈尔滨工业大学 | Device and method for treating chlorophenol wastewater by using ultrasonic-assisted active membrane electrode |
CN111875002A (en) * | 2020-08-04 | 2020-11-03 | 盐城工学院 | Preparation method of microspheric titanium suboxide electrode |
CN113213594A (en) * | 2021-05-28 | 2021-08-06 | 东莞理工学院 | Rare earth metal doped Ti4O7Method for preparing electrode |
CN115947420A (en) * | 2022-06-09 | 2023-04-11 | 松山湖材料实验室 | High-conductivity Magneli-phase titanium suboxide ceramic coating electrode and slurry, preparation method and application thereof |
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