CN109019786A - Preparation method, combination electrode and its application method of MOFs macromolecule combination electrode - Google Patents
Preparation method, combination electrode and its application method of MOFs macromolecule combination electrode Download PDFInfo
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- CN109019786A CN109019786A CN201811065918.9A CN201811065918A CN109019786A CN 109019786 A CN109019786 A CN 109019786A CN 201811065918 A CN201811065918 A CN 201811065918A CN 109019786 A CN109019786 A CN 109019786A
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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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- 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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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- 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
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- 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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- C02F2001/46138—Electrodes comprising a substrate and a coating
- C02F2001/46142—Catalytic coating
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C02F2201/46—Apparatus for electrochemical processes
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Abstract
The invention belongs to electrode technology fields, and in particular to a kind of preparation method, combination electrode material and its application method of MOFs macromolecule combination electrode material.Wherein the preparation method of this combination electrode material is suitable for modifying MOFs macromolecule mixture to electrode surface by way of area load, improves the catalytic oxidation performance of combination electrode material.
Description
Technical field
The present invention relates to electrode technology fields, and in particular to a kind of preparation method of MOFs macromolecule combination electrode material,
Combination electrode material and its application method.
Background technique
Organic pollutant in Electro-catalytic Oxidation Process water body is a kind of efficient, convenient and fast wastewater treatment method.It is urged in electricity
Change in oxidation, Ti electrode is a kind of anode working electrode of commonly selected.Ti electrode anode is due to dimensionally stable, in electrolytic process
Interelectrode distance does not change, it is ensured that electrolysis procedure is carried out in the case where tank voltage is stablized.Meanwhile the work electricity of Ti electrode
It forces down, power consumption is small, and direct current consumption can reduce 10-20%.In addition, Ni―Ti anode long working life, the relatively common sun of corrosion resistance
It is extremely strong, the problems of dissolution of graphite anode and lead anode can be overcome, avoid the pollution to electrolyte and cathode product, and can avoid lead
The deformed short circuit problem of anode improves current efficiency.Ti electrode shape is easy to make, can high precision int, Titanium base is repeatable
It uses.It is with low overpotential characteristic, and the bubble of surface and electrode is easy to exclude between electrode, can effectively reduce electrolyzer electric
Pressure.
But Ti electrode make anode for organic pollutants in water body electrocatalytic oxidation when, it may occur that more analysis oxygen pair
Reaction, this will be greatly reduced the efficiency of catalysis oxidation.Oxygen side reaction is analysed in order to reduce, needs to be surface-treated Ti electrode,
The rate of adsorption for increasing electrode surface and molecule to be degraded, to improve the catalysis oxidation efficiency.
Metal organic framework (MOFs) material is a kind of relatively new porous material, is quickly grown in recent years, and have
Three-dimensional pore structure.Due to the height of metal and organic ligand alternative, and the connection type between metal and ligand is different, makes
It obtains MOFs material and presents structure diversity extremely abundant.MOFs structure also has the order of height simultaneously, to a certain degree
On designability and tailorability, highly developed pore structure make it have superelevation specific surface area.Based on the above spy
Point, MOFs material can be modified on Ti electrode surface to promote its electrocatalytic oxidation efficiency.
But this body structure of MOFs material is very stable, very poor with the compatibility of Ti electrode direct combination, easily in use
It falls off from electrode surface.Therefore, the present invention mixes MOFs material with adhesion agent, and MOFs Material cladding is fixed on titanium to reach
The purpose of electrode surface.Since MOFs material and adhesion agent are all non-conductive, the electricity of electrode can be made if only selecting both materials
Resistance becomes very large and then influences electrode performance, so being also added into a certain amount of conductive agent during compound to reinforce electricity
The transmitting of son.
Based on the above analysis, the present invention has made MOFs macromolecule combination electrode material, and it is organic to be applied to water body
The Electrocatalysis Degradation of pollutant.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of MOFs macromolecule combination electrode material, combination electrode material and
MOFs macromolecule mixture is covered electrode surface by its application method, to promote the catalytic oxidation performance of electrode.
In order to solve the above-mentioned technical problems, the present invention provides a kind of preparation methods of combination electrode material, comprising: passes through
The mode of area load modifies MOFs macromolecule mixture to electrode surface.
Optionally, the electrode is such as, but not limited to Ti electrode, and MOFs macromolecule mixture is covered electrode surface,
Highly developed pore structure makes it have the specific surface area of superelevation, can not only increase the suction of electrode surface Yu molecule to be degraded
Attached rate improves the catalysis oxidation efficiency, can also reduce analysis oxygen side reaction of the Ti electrode in electrocatalytic oxidation, plays protection electricity
The effect of pole substrate.
Further, the method that MOFs macromolecule mixture covers electrode surface may include steps of: step S1,
MOFs material, adhesion agent, conductive agent are mixed in organic solvent, to form MOFs macromolecule mixture；Step S2, will be described
MOFs macromolecule mixture stirs evenly, and with metal stamping and pressing uniform fold in electrode surface；Step S3, surface is covered with
The electrode of MOFs macromolecule mixture, which is put into baking oven, dries.
Optionally, in step s 2, can be stirred under the revolving speed of 60rpm-300rpm by blender 1-60 minutes will
MOFs macromolecule mixture stirs evenly；MOFs macromolecule mixture uniform fold is then taken out in electrode surface.Wherein electrode
The overlay capacity of the MOFs macromolecule mixture on surface is 0.03-0.15mL/cm2。
Optionally, the drying temperature in the step S3 can be true according to the component of MOFs macromolecule mixture, overlay capacity
It is fixed, generally 30-100 DEG C, preferably 40-80 DEG C.
Further, in the MOFs macromolecule mixture: the concentration of the MOFs material is 0.01-0.05g/mL；Institute
The concentration for stating adhesion agent is 0.05-0.20g/mL and the concentration of the conductive agent is 0.05-0.20g/mL.
Optionally, the MOFs material include but is not limited to MIL-53 (Al), MIL-100 (Fe), MIL-101 (Cr),
One or more of metal-organic framework materials such as UIO-66.
Optionally, the adhesion agent is such as, but not limited to high molecular material, can be PTFE (polytetrafluoroethylene (PTFE)), PVDF
At least one of high molecular materials such as (Kynoar), PS (polystyrene), PE (polyethylene).Due to MOFs material itself
Structure is very stable, very poor with the compatibility of Ti electrode direct combination, therefore MOFs material and adhesion agent are blended in organic solvent
Middle formation MOFs macromolecule mixture, is then composite and fixed at Ti electrode surface again, and MOFs material can be effectively prevented and using
It falls off in the process from electrode surface.
Optionally, the conductive agent includes but is not limited to one or more of graphite, graphene, carbon black etc..Due to
MOFs material and adhesion agent are non-conductive, and the conductive agent can be used to improve the electric conductivity of MOFs macromolecule mixture, thus
The resistance of combination electrode material is avoided to become larger.
Optionally, the organic solvent include but is not limited to DMF (dimethylformamide), acetonitrile (dimethylformamide),
One or more of chloroform etc..
In addition, combination electrode material prepared by preparation method of the invention also have the advantage that it is low in cost；Production letter
Just；Electro-catalysis efficiency is obviously improved；Power consumption reduces；Protect anode base material；Extend electrode life；Anode base material can weigh
It is multiple to utilize；Electrode physical property is stablized；It is applicable to electrode base material of various shapes.
Another aspect, the present invention also provides a kind of combination electrode materials, comprising: electrode and is covered on electrode surface
MOFs macromolecule mixture, to improve the catalytic oxidation performance of electrode.Wherein the MOFs macromolecule mixture is suitable for including such as
The substance of respective components in the preparation method of the preceding combination electrode material, details are not described herein.
On the other hand, the present invention also provides a kind of application method of combination electrode material, use combination electrode material for
Anode carries out electrocatalytic oxidation to water body, with the organic pollutant in water body of degrading.Wherein, the combination electrode material can be
Prepared combination electrode material in foregoing preparation method.
Optionally, it is cathode, electricity that graphite electrode can be selected in the application method of the combination electrode material of the application
Current density is 20mA/cm2, pH 9, and select the Na of 0.1mol/L2SO4For electrolyte；And the organic pollutant include but
It is not limited to aniline, phenol etc..
The invention has the advantages that the preparation method of combination electrode material of the invention, by MOFs macromolecule mixture
Cover electrode surface, highly developed pore structure makes it have specific surface area of superelevation, can increase electrode surface with
The rate of adsorption of molecule to be degraded improves the catalysis oxidation efficiency of electrode.
Detailed description of the invention
Present invention will be further explained below with reference to the attached drawings and examples.
Fig. 1 is that the section SEM of pure Ti electrode schemes；
Fig. 2 is the section SEM figure of combination electrode material prepared by embodiment 1；
Fig. 3 is the section SEM figure of combination electrode material prepared by embodiment 2；
Fig. 4 is the section SEM figure of combination electrode material prepared by embodiment 3；
Fig. 5 is the section SEM figure of combination electrode material prepared by embodiment 4；
Fig. 6 is that the surface SEM of pure Ti electrode schemes；
Fig. 7 is the surface SEM figure of combination electrode material prepared by embodiment 1；
Fig. 8 is the surface SEM figure of combination electrode material prepared by embodiment 2；
Fig. 9 is the surface SEM figure of combination electrode material prepared by embodiment 3；
Figure 10 is the surface SEM figure of combination electrode material prepared by embodiment 4；
Figure 11 be embodiment 1-4 preparation combination electrode material electrocatalytic oxidation of phenylamine experiment in aniline residual concentration at any time
Between variation diagram；
Figure 12 is ln (initial concentration/instant in the combination electrode material electrocatalytic oxidation of phenylamine experiment of embodiment 1-4 preparation
Concentration) change with time figure；
Figure 13 be embodiment 1-4 preparation combination electrode material electrocatalytic oxidation phenol experiment in phenol residual concentration at any time
Between variation diagram；
Figure 14 is ln (initial concentration/instant in the combination electrode material electrocatalytic oxidation phenol experiment of embodiment 1-4 preparation
Concentration) change with time figure.
Specific embodiment
In conjunction with the accompanying drawings, the present invention is further explained in detail.
In this application, the concentration of component of the MOFs macromolecule mixture in the preparation method of combination electrode material and covering
Amount can be there are many embodiment, as shown in table 1.But (it is mixed that surface does not cover MOFs macromolecule with pure Ti electrode due to needing
Close object Ti electrode) make catalysis oxidation Organic Pollutants In Water (aniline, phenol etc.) contrasting detection test, MOFs macromolecule
Mixture and its overlay capacity need to keep close or identical, to guarantee the reliability of testing result, now only enumerate part embodiment party
The specific implementation process of the preparation method of the combination electrode material of formula, as shown in embodiment 1-4.
Each component concentration and overlay capacity in 1 MOFs macromolecule mixture of table
Embodiment 1
Take MIL-53 (Al) 0.1g, PTFE 1g, carbon black 2g in 10mL volumetric flask, with being poured into beaker after DMF constant volume,
It is stirred 15 minutes under 140rpm revolving speed, takes 0.3mL mixed liquor metal stamping and pressing uniform fold on the Ti electrode of 4cm × 1cm,
It is dried at 38 DEG C.Section (Fig. 2) and surface (Fig. 7) to the combination electrode material to complete do sem test, and with
The section (Fig. 1) and surface (Fig. 6) of pure Ti electrode compare.Relative to pure Ti electrode, the combination electrode material table of embodiment 1
There is apparent MOFs crystalline texture in face, and section can be seen that one layer of increased decorative layer, can determine combination electrode material system
Standby success.
Embodiment 2
It takes MIL-100 (Fe) 0.3g, PVDF 1.5g, graphite 1.5g in 10mL volumetric flask, is poured into after after acetonitrile constant volume
Beaker stirs 26 minutes under 200rpm revolving speed, takes 1.6mL mixed liquor metal stamping and pressing uniform fold in the titanium electricity of 4cm × 4cm
On extremely, dried at 55 DEG C.Sem test is done to the section (Fig. 3) and surface (Fig. 8) of the combination electrode material to complete,
And it is compared with the section of pure Ti electrode (Fig. 1) and surface (Fig. 6).Relative to pure Ti electrode, the combination electrode material of embodiment 2
There is apparent MOFs crystalline texture on material surface, and section can be seen that one layer of increased decorative layer, can determine combination electrode material
Material is successfully prepared.
Embodiment 3
It takes MIL-101 (Cr) 0.4g, PE 0.5g, graphene 0.5g in 10mL volumetric flask, is fallen with after chloroform constant volume
Enter beaker, stirred 48 minutes under 240rpm revolving speed, takes 2.5mL mixed liquor metal stamping and pressing uniform fold 4cm × 10cm's
On Ti electrode, dried at 66 DEG C.Scanning electron microscope is done to the section (Fig. 4) and surface (Fig. 9) of the combination electrode material to complete
Test, and compared with the section of pure Ti electrode (Fig. 1) and surface (Fig. 6).Relative to pure Ti electrode, embodiment 3 it is compound
Electrode material surface has apparent MOFs crystalline texture, and section can be seen that one layer of increased decorative layer, can determine compound
Electrode material is successfully prepared.
Embodiment 4
UIO-66 0.5g is taken, PVDF2g, graphene 1g are in 10mL volumetric flask, with pouring into beaker after dimethyl sulfoxide constant volume,
It is stirred 55 minutes under 290rpm revolving speed, takes 5.3mL mixed liquor metal stamping and pressing uniform fold in the Ti electrode plate of 6cm × 10cm
On, it is dried at 78 DEG C.Sem test is done to the section (Fig. 5) and surface (Figure 10) of the combination electrode material to complete,
And it is compared with the section of pure Ti electrode (Fig. 1) and surface (Fig. 6).Relative to pure Ti electrode, the combination electrode material of embodiment 4
There is apparent MOFs crystalline texture on material surface, and section can be seen that one layer of increased decorative layer, can determine combination electrode material
Material is successfully prepared.
Embodiment 5
The combination electrode material that embodiment 1-4 preparation is respectively adopted is that the aniline that anode carries out in electrocatalytic oxidation water body is real
It tests, and is compared with pure Ti electrode for the case where anode.Wherein, current density 20mA/cm2, pH 9,0.1mol/L's
Na2SO4For electrolyte, the initial concentration of aniline is 100ppm.
As is illustrated by figs. 11 and 12, the aniline of the combination electrode material Electrocatalysis Degradation of the preparation method preparation of the application is dense
Spend that the pure Ti electrode of suppression ratio is fast, and the reaction rate constant of catalysis oxidation is also bigger than pure Ti electrode, therefore combination electrode material is urged
Change oxidation susceptibility to get a promotion.Simultaneously it can also be seen that in the case where meeting the requirement of electrode beam conduction, combination electrode material
Material is positively correlated MOFs material content in the electrocatalytic oxidation property and combination electrode material of aniline, i.e. MOFs macromolecule mixture
Middle MOFs material concentration is higher, and the catalytic oxidation performance of combination electrode material is better；And with the extension of catalysis oxidation time,
MOFs material concentration is higher, and the promotion effect of the catalytic oxidation performance of combination electrode material is more obvious.
Embodiment 6
The combination electrode material for using embodiment 1-4 to prepare carries out the phenol experiment in electrocatalytic oxidation water body for anode,
And it is compared with pure Ti electrode for the case where anode.Current density is 20mA/cm2, the Na of pH 9,0.1mol/L2SO4For electricity
Liquid is solved, the initial concentration of phenol is 100ppm.As shown in Figure 13 and Figure 14, the combination electrode material of the preparation method preparation of the application
Expect that the pure Ti electrode of phenol concentration suppression ratio of Electrocatalysis Degradation is fast, the reaction rate constant of catalysis oxidation is also bigger than pure Ti electrode,
Therefore the catalytic oxidation performance of combination electrode material gets a promotion.Meanwhile as seen from Figure 14, meeting electrode beam conduction
Property require in the case where, MOFs material content in the electrocatalytic oxidation property and combination electrode material of combination electrode material Pyrogentisinic Acid
It is positively correlated, i.e., MOFs material concentration is higher in MOFs macromolecule mixture, and the catalytic oxidation performance of combination electrode material is better；And
And with the extension of catalysis oxidation time, MOFs material concentration is higher, the promotion effect of the catalytic oxidation performance of combination electrode material
Fruit is more obvious.
In conclusion the preparation method of the combination electrode material of the application is by way of area load by MOFs macromolecule
To electrode surface, highly developed pore structure makes it have specific surface area of superelevation for mixture modification, can increase electrode
The rate of adsorption on surface and molecule to be degraded improves the catalysis oxidation efficiency of combination electrode material；It is improved by conductive agent
The electric conductivity of MOFs macromolecule mixture avoids the resistance of combination electrode material from becoming larger, so that the electric conductivity for meeting electrode is wanted
It asks；MOFs material, conductive agent are mixed by adhesion agent and form MOFs macromolecule mixture in organic solvent, is increased and titanium
The compatibility of electrode not only can be effectively prevented MOFs macromolecule mixture and fall off in use from electrode surface, may be used also
With guard electrode substrate, extend electrode life.
Taking the above-mentioned ideal embodiment according to the present invention as inspiration, through the above description, relevant staff is complete
Various changes and amendments can be carried out without departing from the scope of the technological thought of the present invention' entirely.The technology of this invention
Property range is not limited to the contents of the specification, it is necessary to which the technical scope thereof is determined according to the scope of the claim.
Claims (10)
1. a kind of preparation method of combination electrode material characterized by comprising
MOFs macromolecule mixture is modified to electrode surface by way of area load.
2. preparation method according to claim 1, which is characterized in that
It is described to include: by the method for MOFs macromolecule mixture modification to electrode surface by way of area load
MOFs material, adhesion agent, conductive agent are mixed in organic solvent, to form the MOFs macromolecule mixture；
The MOFs macromolecule mixture is stirred evenly, and uniform fold is in electrode surface；And
Surface is covered with to the electrode drying of MOFs macromolecule mixture.
3. preparation method according to claim 2, which is characterized in that
The drying temperature of the electrode is 30-100 DEG C.
4. preparation method according to claim 2, which is characterized in that
In the MOFs macromolecule mixture:
The concentration of the MOFs material is 0.01-0.05g/mL；
The concentration of the adhesion agent is 0.05-0.20g/mL；And
The concentration of the conductive agent is 0.05-0.20g/mL.
5. preparation method according to claim 2, which is characterized in that
The MOFs material is the one or more of MIL-53 (Al), MIL-100 (Fe), MIL-101 (Cr), UIO-66.
6. preparation method according to claim 2, which is characterized in that
The adhesion agent is high molecular material, i.e.,
The adhesion agent is one or more of PTFE, PVDF, PS, PE.
7. preparation method according to claim 2, which is characterized in that
The conductive agent is one or more of graphite, graphene, carbon black.
8. preparation method according to claim 2, which is characterized in that
The organic solvent is one or more of DMF, acetonitrile, chloroform.
9. a kind of combination electrode material characterized by comprising
Electrode and the MOFs macromolecule mixture for being covered on electrode surface；
The MOFs macromolecule mixture is suitable for including such as respective components in the described in any item preparation methods of claim 1-8
Substance.
10. a kind of application method of combination electrode material, which is characterized in that
Combination electrode material is used to carry out electrocatalytic oxidation to water body for anode, with the organic pollutant in water body of degrading.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110172709A (en) * | 2019-06-05 | 2019-08-27 | 中南大学 | The preparation method and application of MOFs char-forming material electrochemical cathode based on metal ion and organic matter absorption |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110172709A (en) * | 2019-06-05 | 2019-08-27 | 中南大学 | The preparation method and application of MOFs char-forming material electrochemical cathode based on metal ion and organic matter absorption |
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Application publication date: 20181218 |