CN108796550A - A kind of preparation method of graphene and carbon nanotube modified synergic membrane electrode - Google Patents
A kind of preparation method of graphene and carbon nanotube modified synergic membrane electrode Download PDFInfo
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- CN108796550A CN108796550A CN201810533769.8A CN201810533769A CN108796550A CN 108796550 A CN108796550 A CN 108796550A CN 201810533769 A CN201810533769 A CN 201810533769A CN 108796550 A CN108796550 A CN 108796550A
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B1/00—Electrolytic production of inorganic compounds or non-metals
- C25B1/01—Products
- C25B1/13—Ozone
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
- C25B11/04—Electrodes; Manufacture thereof not otherwise provided for characterised by the material
- C25B11/051—Electrodes formed of electrocatalysts on a substrate or carrier
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
- C25B11/04—Electrodes; Manufacture thereof not otherwise provided for characterised by the material
- C25B11/051—Electrodes formed of electrocatalysts on a substrate or carrier
- C25B11/073—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material
- C25B11/091—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material consisting of at least one catalytic element and at least one catalytic compound; consisting of two or more catalytic elements or catalytic compounds
Abstract
The present invention provides the preparation methods of a kind of graphene and carbon nanotube modified synergic membrane electrode, include the following steps：（1）Graphene is modified；（2）Carbon nano-tube modification；（3）Doping；（4）Film；（5）Dipping；（6）Oxidation, contact of the film with catalyst is close, and catalyst granules is fine and closely woven, can obtain better catalytic effect, so that the formation efficiency of ozone is improved, and is added to graphene and carbon nanotube, and the two collaboration improves the catalysis efficiency of membrane electrode.
Description
Technical field
The present invention relates to the preparation methods of a kind of graphene and carbon nanotube modified synergic membrane electrode, mainly for the preparation of smelly
Oxygen, specific is using the method for preparing membrane electrode through silane coupler modified graphene and carbon nanotube.
Background technology
Electrolysis, which prepares ozone, to be had the advantages that the ozoniferous concentration of production is high, does not generate nitrogen oxides, smelly to prepare at present
The method of oxygen first choice.And the preparation that a critical component of electrolysis is compound film electrode, existing preparation method includes hot pressing
Method and electrochemical deposition method, but the catalyst granules that pressure sintering is unable to get is larger, and activity is relatively low, and electrochemical deposition method is electroplated
It is affected.Moreover, existing membrane electrode catalytic activity is low, it is necessary to be further improved.
Invention content
In order to solve the problem above-mentioned, the present invention proposes a kind of system for the graphene modification membrane electrode being used to prepare ozone
Preparation Method, compared to the prior art, contact of the film with catalyst is close, and catalyst granules is fine and closely woven, can be preferably catalyzed
Effect so that the formation efficiency of ozone is improved, and is added to graphene and carbon nanotube, it is desirable to which the two collaboration changes
The catalysis efficiency of kind membrane electrode.
Technical scheme is as follows：
A kind of preparation method of graphene and carbon nanotube modified synergic membrane electrode, includes the following steps：
（1）Graphene is modified
A certain amount of graphene oxide is taken, is distributed in absolute ethyl alcohol, ultrasound 1-30min, forms 1-15g/L's under certain power
Dispersion liquid is added amino silicane coupling agent, reacts 1-12h under mechanical agitation, mixing speed 400-800rpm obtains silane and changes
The graphene of property；
（2）Carbon nano-tube modification
A certain amount of carbon nanotube is taken, is distributed in absolute ethyl alcohol, Fenton reagent is added and carries out hydroxylating processing, it is then ultrasonic
5-10min forms the dispersion liquid of 0.5-8g/L, and amino silicane coupling agent is added, reacts 1-12h, mixing speed under mechanical agitation
For 400-800rpm, silane-modified carbon nanotube is obtained；
（3）Doping
Perfluorosulfonic acid ion exchanger resin is dissolved into organic solution, modified graphene and carbon nanometer are slowly added under stirring
Pipe, ultrasound 5-20min, obtains the mixed liquor of doped graphene and graphene after addition；
（4）Film
Tetrafluoroethene container is taken, SPE films are placed in bottom, is uniformly poured on SPE films and covers doped graphene and carbon nanotube
Mixed liquor waits for that solvent volatilizees, and it is that SPE films, upper layer are compound for the exchange film layer containing graphene and carbon nanotube to form bottom
Film；
（5）Dipping
By the Pb (NO of 0.1-1mol/L3)2It is configured to maceration extract, step with the NaF of 5-200mmol/L（4）Obtained composite membrane
It keeps flat, will be immersed in maceration extract containing the exchange film layer of graphene and carbon nanotube, dip time 1-10h, after the completion of dipping,
It is washed with deionized, the composite membrane after being impregnated；
（6）Oxidation
The NaOH or KOH solution for preparing 1-6mol/L are added in the composite membrane merging solution after dipping oxidant, aoxidize 1-
5h, obtaining deposition has β-PbO2Composite membrane.
Step（1）In ultrasonic power be 10-60W, the preferred 2-10min of ultrasonic time.
Step（1）In the preferred 5-10g/L of graphene concentration.
Step（2）In the preferred 1-5g/L of carbon nanotube concentration.
Step（1）And/or（2）In, the amino silicane coupling agent in KH550, KH540, KH972, KH552 one
Kind is a variety of.
Step（4）In SPE films be selected from Nafion series membranes, preferably Nafion 324.
The SPE films and the thickness ratio of exchange film layer containing graphene are 10-1:1, preferably 5-2:1.
Step（5）In, the Pb (NO3)2Concentration preferred 0.2-0.8mol/L, more preferable 0.3-0.5mol/L.
The preferred 10-20mmol/L of NaF concentration.
The membrane electrode obtained by above-mentioned dipping-oxidizing process, contact of the film with catalyst is close, and catalyst granules is fine and closely woven,
Better catalytic effect can be obtained, so that the formation efficiency of ozone is improved.
The bi-dimensional cellular shape structure that graphene is made of single layer of carbon atom, basic structural unit be organic material in most
Stable six-membered ring structure has good chemical stability, is the Typical Representative of two-dimension nano materials, and graphene also has excellent
Good electric property and catalytic performance.
Carbon nanotube is as monodimension nanometer material, and light-weight, hexagonal structure connection is perfect, has many abnormal power
, electricity and chemical property, hardness and the diamond phase of carbon nanotube are worked as, and but possess good flexibility, carbon nanotube has
Good electric conductivity, since the structure of carbon nanotube and the lamellar structure of graphite are identical, so having good electric property.
Therefore, by graphene and carbon nanotube for when being modified lead dioxide electrode, the catalysis of electrode can be obviously improved
Performance improves the formation efficiency of ozone, and can be obviously improved the service life of electrode.Moreover, the two dimension of graphene
The one-dimentional structure of structure and carbon nanotube is combined, and compound to a certain extent to become tridimensional network, the two is urged electrode
Change and show excellent synergy in effect, improves the catalytic performance of electrode jointly.
But the compatibility performance of graphene, carbon nanotube and membrane electrode is bad, leads to the film for adding graphene and carbon nanotube
Electrode cannot play the effect of graphene to the greatest extent.The present invention is first to graphene and carbon nanotube addition amino silane coupling
Agent is modified, and is reacted using the sulfonic acid group in modified exposed amino and perfluorosulfonic acid ion exchanger resin, to essence
Solve the above problem.
Specific implementation mode
Below in conjunction with specific embodiment, the present invention is described in detail.
Embodiment 1：
A kind of preparation method of graphene and carbon nanotube modified synergic membrane electrode, includes the following steps：
（1）Graphene is modified
A certain amount of graphene oxide is taken, is distributed in absolute ethyl alcohol, ultrasound 10min, forms the dispersion liquid of 10g/L, add under 50W
Enter amino silicane coupling agent KH550,2h is reacted under mechanical agitation, mixing speed 500rpm obtains silane-modified graphene；
（2）Carbon nano-tube modification
A certain amount of carbon nanotube is taken, is distributed in absolute ethyl alcohol, Fenton reagent is added and carries out hydroxylating processing, it is then ultrasonic
8min forms the dispersion liquid of 5g/L, and amino silicane coupling agent is added, reacts 2h under mechanical agitation, mixing speed 500rpm is obtained
To silane-modified carbon nanotube；
（3）Doping
Perfluorosulfonic acid ion exchanger resin is dissolved into organic solution, modified graphene and carbon nanometer are slowly added under stirring
Pipe, ultrasound 10min, obtains the mixed liquor of doped graphene and graphene after addition；
（4）Film
Tetrafluoroethene container is taken, SPE films are placed in bottom, is uniformly poured on SPE films and covers doped graphene and carbon nanotube
Mixed liquor waits for that solvent volatilizees, and it is that SPE films, upper layer are compound for the exchange film layer containing graphene and carbon nanotube to form bottom
Film；
（5）Dipping
By the Pb (NO of 0.6mol/L3)2It is configured to maceration extract, step with the NaF of 20mmol/L（4）Obtained composite membrane is kept flat,
It will be immersed in maceration extract containing the exchange film layer of graphene and carbon nanotube, dip time 6h, after the completion of dipping, use deionization
Water washing, the composite membrane after being impregnated；
（6）Oxidation
The NaOH solution for preparing 4mol/L is added in the composite membrane merging solution after dipping oxidant, aoxidizes 2h, sunk
Product has β-PbO2Composite membrane.
After tested, β-PbO2Content be respectively 80.46mg/cm2, the overpotential for oxygen evolution of electrode is 1960mV, current density
30mA/cm2Under current efficiency be 28.94%, accelerated service life be 2.25 hours（About 234 days actual lives）.
Comparative example 1：
A kind of preparation method of graphene and carbon nanotube modified synergic membrane electrode, includes the following steps：
（1）Graphene prepares
A certain amount of graphene oxide is taken, is distributed in absolute ethyl alcohol, ultrasound 10min, forms the dispersion liquid of 10g/L, machine under 50W
Tool stirs 2h, mixing speed 500rpm, the graphene disperseed；
（2）Carbon nanotube prepares
A certain amount of carbon nanotube is taken, is distributed in absolute ethyl alcohol, then ultrasound 8min, forms the dispersion liquid of 5g/L, machinery stirs
Mix 2h, mixing speed 500rpm, the carbon nanotube disperseed；
（3）Doping
Perfluorosulfonic acid ion exchanger resin is dissolved into organic solution, the graphene and carbon nanometer of dispersion are slowly added under stirring
Pipe, ultrasound 10min, obtains the mixed liquor of doped graphene and graphene after addition；
（4）Film
Tetrafluoroethene container is taken, SPE films are placed in bottom, is uniformly poured on SPE films and covers doped graphene and carbon nanotube
Mixed liquor waits for that solvent volatilizees, and it is that SPE films, upper layer are compound for the exchange film layer containing graphene and carbon nanotube to form bottom
Film；
（5）Dipping
By the Pb (NO of 0.6mol/L3)2It is configured to maceration extract, step with the NaF of 20mmol/L（4）Obtained composite membrane is kept flat,
It will be immersed in maceration extract containing the exchange film layer of graphene and carbon nanotube, dip time 6h, after the completion of dipping, use deionization
Water washing, the composite membrane after being impregnated；
（6）Oxidation
The NaOH solution for preparing 4mol/L is added in the composite membrane merging solution after dipping oxidant, aoxidizes 2h, sunk
Product has β-PbO2Composite membrane.
After tested, β-PbO2Content be respectively 78.95mg/cm2, the overpotential for oxygen evolution of electrode is 1907mV, current density
30mA/cm2Under current efficiency be 24.18%, accelerated service life be 2.20 hours（About 228 days actual lives）.
Comparative example 2：
A kind of graphene is modified the preparation method of membrane electrode, includes the following steps：
（1）Graphene is modified
A certain amount of graphene oxide is taken, is distributed in absolute ethyl alcohol, ultrasound 10min, forms the dispersion liquid of 10g/L, add under 50W
Enter amino silicane coupling agent KH550,2h is reacted under mechanical agitation, mixing speed 500rpm obtains silane-modified graphene；
（2）Doping
Perfluorosulfonic acid ion exchanger resin is dissolved into organic solution, modified graphene is slowly added under stirring, has been added
Ultrasound 10min, obtains the mixed liquor of doped graphene after finishing；
（3）Film
Tetrafluoroethene container is taken, SPE films are placed in bottom, the mixed liquor for covering doped graphene is uniformly poured on SPE films, are waited for molten
Agent is volatilized, and it is SPE films, the composite membrane that upper layer is the exchange film layer containing graphene to form bottom；
（4）Dipping
By the Pb (NO of 0.6mol/L3)2It is configured to maceration extract, step with the NaF of 20mmol/L（3）Obtained composite membrane is kept flat,
Exchange film layer containing graphene is immersed in maceration extract, dip time 6h, after the completion of dipping, is washed with deionized, obtains
Composite membrane after to dipping；
（5）Oxidation
The NaOH solution for preparing 4mol/L is added in the composite membrane merging solution after dipping oxidant, aoxidizes 2h, sunk
Product has β-PbO2Composite membrane.
After tested, β-PbO2Content be respectively 79.02mg/cm2, the overpotential for oxygen evolution of electrode is 1989mV, current density
30mA/cm2Under current efficiency be 21.01%, accelerated service life be 2.06 hours（About 214 days actual lives）.
Comparative example 3：
A kind of preparation method of carbon nanotube modified synergic membrane electrode, includes the following steps：
（1）Carbon nano-tube modification
A certain amount of carbon nanotube is taken, is distributed in absolute ethyl alcohol, Fenton reagent is added and carries out hydroxylating processing, it is then ultrasonic
8min forms the dispersion liquid of 5g/L, and amino silicane coupling agent is added, reacts 2h under mechanical agitation, mixing speed 500rpm is obtained
To silane-modified carbon nanotube；
（2）Doping
Perfluorosulfonic acid ion exchanger resin is dissolved into organic solution, modified graphene and carbon nanometer are slowly added under stirring
Pipe, ultrasound 10min, obtains the mixed liquor of doped graphene and graphene after addition；
（3）Film
Tetrafluoroethene container is taken, SPE films are placed in bottom, is uniformly poured on SPE films and covers doped graphene and carbon nanotube
Mixed liquor waits for that solvent volatilizees, and it is that SPE films, upper layer are compound for the exchange film layer containing graphene and carbon nanotube to form bottom
Film；
（4）Dipping
By the Pb (NO of 0.6mol/L3)2It is configured to maceration extract, step with the NaF of 20mmol/L（3）Obtained composite membrane is kept flat,
It will be immersed in maceration extract containing the exchange film layer of graphene and carbon nanotube, dip time 6h, after the completion of dipping, use deionization
Water washing, the composite membrane after being impregnated；
（5）Oxidation
The NaOH solution for preparing 4mol/L is added in the composite membrane merging solution after dipping oxidant, aoxidizes 2h, sunk
Product has β-PbO2Composite membrane.
After tested, β-PbO2Content be respectively 77.88mg/cm2, the overpotential for oxygen evolution of electrode is 2001mV, current density
30mA/cm2Under current efficiency be 20.85%, accelerated service life be 2.02 hours（About 210 days actual lives）.
From the comparison of embodiment 1 and comparative example 1 can be seen that graphene and carbon nanotube it is not modified when, electrode is urged
Change ineffective, current efficiency is relatively low.Individually addition graphene or carbon are can be seen that from the comparison of embodiment 1 and comparative example 2-3
The catalytic efficiency of nanotube is general, but the two also has simultaneously added with apparent synergy, and to the service life of electrode
Certain improvement, this may be the tridimensional network to be formed, and cause to have on its electricity, catalytic performance and mechanics bright
Aobvious improvement.
Claims (9)
1. the preparation method of a kind of graphene and carbon nanotube modified synergic membrane electrode, which is characterized in that include the following steps：
（1）Graphene is modified
A certain amount of graphene oxide is taken, is distributed in absolute ethyl alcohol, ultrasound 1-30min, forms 1-15g/L's under certain power
Dispersion liquid is added amino silicane coupling agent, reacts 1-12h under mechanical agitation, mixing speed 400-800rpm obtains silane and changes
The graphene of property；
（2）Carbon nano-tube modification
A certain amount of carbon nanotube is taken, is distributed in absolute ethyl alcohol, Fenton reagent is added and carries out hydroxylating processing, it is then ultrasonic
5-10min forms the dispersion liquid of 0.5-8g/L, and amino silicane coupling agent is added, reacts 1-12h, mixing speed under mechanical agitation
For 400-800rpm, silane-modified carbon nanotube is obtained；
（3）Doping
Perfluorosulfonic acid ion exchanger resin is dissolved into organic solution, modified graphene and carbon nanometer are slowly added under stirring
Pipe, ultrasound 5-20min, obtains the mixed liquor of doped graphene and graphene after addition；
（4）Film
Tetrafluoroethene container is taken, SPE films are placed in bottom, is uniformly poured on SPE films and covers doped graphene and carbon nanotube
Mixed liquor waits for that solvent volatilizees, and it is that SPE films, upper layer are compound for the exchange film layer containing graphene and carbon nanotube to form bottom
Film；
（5）Dipping
By the Pb (NO of 0.1-1mol/L3)2It is configured to maceration extract, step with the NaF of 5-200mmol/L（4）Obtained composite membrane is flat
It puts, will be immersed in maceration extract containing the exchange film layer of graphene and carbon nanotube, dip time 1-10h, after the completion of dipping, used
Deionized water is washed, the composite membrane after being impregnated；
（6）Oxidation
The NaOH or KOH solution for preparing 1-6mol/L are added in the composite membrane merging solution after dipping oxidant, aoxidize 1-
5h, obtaining deposition has β-PbO2Composite membrane.
2. according to the method described in claim 1, it is characterized in that, step（1）In ultrasonic power be 10-60W, ultrasonic time
It is preferred that 2-10min.
3. according to the method described in claim 1, it is characterized in that, step（1）In the preferred 5-10g/L of graphene concentration.
4. according to the method described in claim 1, it is characterized in that, step（2）In the preferred 1-5g/L of carbon nanotube concentration.
5. according to the method described in claim 1, it is characterized in that, step（1）And/or（2）In, the amino silicane coupling agent
It is one or more in KH550, KH540, KH972, KH552.
6. according to the method described in claim 1, it is characterized in that, step（4）In SPE films be selected from Nafion series membranes, it is excellent
Select Nafion 324.
7. according to the method described in claim 1, it is characterized in that, the thickness of the SPE films and the exchange film layer containing graphene
Degree is than being 10-1:1, preferably 5-2:1.
8. according to the method described in claim 1, it is characterized in that, step（5）In, the Pb (NO3)2The preferred 0.2- of concentration
0.8mol/L, more preferable 0.3-0.5mol/L.
9. according to the method described in claim 1, it is characterized in that, the preferred 10-20mmol/L of NaF concentration.
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| CN113113622A (en) * | 2021-03-16 | 2021-07-13 | 国家电投集团氢能科技发展有限公司 | Fuel cell catalyst layer slurry and preparation method and application thereof |
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