CN105836855B - A kind of preparation method and application of graphene gas-diffusion electrode - Google Patents
A kind of preparation method and application of graphene gas-diffusion electrode Download PDFInfo
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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
- C02F1/72—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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- 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
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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
- C02F2001/46157—Perforated or foraminous electrodes
- C02F2001/46161—Porous electrodes
- C02F2001/46166—Gas diffusion 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
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
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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
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/02—Specific form of oxidant
- C02F2305/023—Reactive oxygen species, singlet oxygen, OH radical
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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
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/02—Specific form of oxidant
- C02F2305/026—Fenton's reagent
Abstract
The present invention relates to electrode material preparation technical fields, and in particular to a kind of preparation method and application of graphene gas-diffusion electrode.Its specific preparation process is as follows: by crystalline flake graphite, NaNO3It is mixed in ice bath with the concentrated sulfuric acid, and and KMnO4After slow reaction, appropriate 30% H is added2O2Sufficiently reaction, filtering are dry after washing to neutrality.Product ultrasound in aqueous solution obtains dispersion liquid, adjusts pH, upper layer stabilizing solution is taken after centrifugation, appropriate hydrazine hydrate is added and obtains graphene dispersing solution.The dispersion liquid is uniformly mixed with graphite powder, ethyl alcohol, polytetrafluoroethylene (PTFE) lotion.Constant temperature water bath is attached on stainless (steel) wire when being in sticky paste to the mixture, is pressed into graphene gas-diffusion electrode.For the present invention in electricity-Fenton-like system, oxidability is stronger, can be used in all kinds of processing containing organic pollutant wastewater.
Description
Technical field
The present invention relates to technical field of sewage, and in particular to a kind of preparation method of graphene gas-diffusion electrode and
Its application method.
Background technique
The one kind of electricity-Fenton process as high-level oxidation technology, because of its thorough, high-efficient, easy to operate, time consumption and energy consumption of degradation
It is few, by the common concern of people in environment protection field, it is widely used in the processing containing organic pollutant wastewater.In order to improve
Cathode is to the catalytic activity of two electronic reduction reactions of dissolved oxygen in electricity-Fenton-like system, promote electric Fenton oxidation technology into one
Step development, the preparation of electrode material and the new hot spot for being selected to the area research.Cathode used in traditional electricity-Fenton-like system
Material is mainly graphite, activated carbon or activated carbon fibre etc., and the catalytic activity of such electrode is not high enough, and current efficiency is lower, because
The application of this electricity-Fenton process is by certain restriction.
Summary of the invention
The purpose of the present invention is to provide the preparation methods and application of a kind of graphene gas-diffusion electrode, to improve electricity-
The catalytic activity and current efficiency of electrode in Fenton-like system.
To achieve the goals above, present invention provide the technical scheme that a kind of preparation of graphene gas-diffusion electrode
Method includes the following steps:
Step (1): by crystalline flake graphite, NaNO3With the concentrated sulfuric acid in the ratio of 3.0 g: 1.5 ~ 2g: 160 mL in ice-water bath
1 h of middle reaction, then weigh 9.0437 g KMnO4In being slowly added to beaker in 3 h dropwise, 2 h are reacted；
Step (2): removing ice-water bath, is warming up to 40 DEG C or so, continues to be stirred to react 1.5 h；It is slowly added to 160 mL steaming
Distilled water is heated to boiling, and is stirred to react 1 h；
Step (3): the resulting mixed solution of step 2 is placed into a period of time, in 48-52 DEG C plus 30 mL 30% of H2O2,
175 mL distilled water are added, react 3 h, cooled and filtered；With mass fraction be 30% salt acid elution to sulfate radical-free until,
It is washed with distilled water to PH=7 again, filter residue is dried in vacuo in 40 DEG C, and graphene oxide is made；
Step (4): weighing 100.0 mg ultrasound in 100 mL aqueous solutions for the resulting graphene oxide of step 3, until
Obtain the stable dispersions almost without obvious particle；The ammonium hydroxide that mass fraction is 28% is taken to adjust the pH to 10 of dispersion liquid；
Step (5): by the resulting solution of step 4 in 4000 rmin-1It is unstripped that 3 min of lower centrifugation remove minute quantity
Graphite oxide is added 0.2mL hydrazine hydrate into the graphene oxide dispersion after centrifugation and obtains graphite in 90 DEG C of 2 h of reaction
Alkene dispersion liquid;
Step (6): it takes 0.8 g graphite and 160 mL, 3% alcohol mixture in room temperature 10 min of ultrasound, adds obtained by step 5
10 ~ 30 mL of graphene dispersing solution and 0.2 g polytetrafluoroethylene (PTFE) room temperature 15 min of ultrasound, in water-bath constant temperature 80
DEG C it is heated to paste taking-up；
Step (7): nickel screen two sides are uniformly attached to after the resulting pasty mixture of step 6 is slightly cooling, place one section
After time mushy freezing, cold pressing 3 min molding (with a thickness of 0.5-0.7 mm), in 300 DEG C of Muffle furnace 1.5 h of calcining to get
Graphene gas-diffusion electrode.
Application of the graphene gas-diffusion electrode that above-mentioned preparation method obtains in electricity-Fenton-like system.
Application method of the graphene gas-diffusion electrode that above-mentioned preparation method obtains in electricity-Fenton-like system, before use,
Electrode impregnates 24 h in acetone, to remove the surface reactive material in its ethyl alcohol remained on surface and PTFE, finally spend from
Sub- water repeated flushing is simultaneously dried, and is accessed and is used according to the method for conventional electrodes.
Compared with prior art, the invention has the advantages that
1, the present invention made by be it is a kind of by graphene adulterate gas-diffusion electrode, compared to common gases spread electricity
Pole, the catalysis characteristics and high-specific surface area of graphene itself provide more excellent reaction condition for graphene gas-diffusion electrode
And place, to show higher catalytic activity and current efficiency in electricity-Fenton-like system；
2, in calcination process, polytetrafluoro volume reduces, and electrode porosity itself increases, to make the electrode in electricity-Fenton
Increase in reaction process with effective contact area of solution, promotes the raw H of electricity2O2Yield increases, and effectively increases hydroxyl radical free radical
Formation efficiency enhances the oxidability of system；
3, applied widely: to can be used in all kinds of processing containing organic pollutant wastewater.
Detailed description of the invention
Fig. 1 is graphene gas-diffusion electrode material object photo prepared by embodiment 2；
Fig. 2 is the scanning electron microscope (SEM) of graphene gas-diffusion electrode prepared by embodiment 2；
Fig. 3 is for 2 Different electrodes of embodiment to rhodamine B degradation efficiency in electricity-Fenton-like system.(CP: conventional carbon electricity
Pole；DGE: graphene gas-diffusion electrode).
Specific embodiment
The present invention is described in detail below in conjunction with drawings and examples.
Embodiment 1:
A kind of preparation method of graphene gas-diffusion electrode, includes the following steps:
Step (1): by crystalline flake graphite, NaNO3With the concentrated sulfuric acid in the ratio of 3.0 g: 1.5 g: 160 mL in ice-water bath
1 h is reacted, then weighs 9.0437 g KMnO4In being slowly added to beaker in 3 h dropwise, 2 h are reacted;
Step (2): removing ice-water bath, is warming up to 40 DEG C or so, continues to be stirred to react 1.5 h.It is slowly added to 160 mL steaming
Distilled water is heated to boiling, and is stirred to react 1 h;
Step (3): the resulting mixed solution of step 2 is placed into a period of time, in 48-52 DEG C plus 30 mL 30% of H2O2,
175 mL distilled water are added, react 3 h, cooled and filtered.With mass fraction be 30% salt acid elution to sulfate radical-free until,
It is washed with distilled water to PH=7 again.Filter residue is dried in vacuo in 40 DEG C, and graphene oxide is made;
Step (4): weighing 100.0 mg ultrasound in 100 mL aqueous solutions for the resulting graphene oxide of step 3, until
Obtain the stable dispersions almost without obvious particle.The ammonium hydroxide that mass fraction is 28% is taken to adjust the pH to 10 of dispersion liquid;
Step (5): by the resulting solution of step 4 in 4000 rmin-1It is unstripped that 3 min of lower centrifugation remove minute quantity
Graphite oxide is added 0.2mL hydrazine hydrate into the graphene oxide dispersion after centrifugation and obtains graphite in 90 DEG C of 2 h of reaction
Alkene dispersion liquid;
Step (6): it takes 0.8 g graphite and 160 mL, 3% alcohol mixture in room temperature 10 min of ultrasound, adds obtained by step 5
30 mL of graphene dispersing solution and 0.2 g polytetrafluoroethylene (PTFE) room temperature 15 min of ultrasound, at 80 DEG C of water-bath constant temperature plus
Heat to paste takes out;
Step (7): nickel screen two sides are uniformly attached to after the resulting pasty mixture of step 6 is slightly cooling, place one section
After time mushy freezing, cold pressing 3 min molding (with a thickness of 0.7 mm), in 300 DEG C of Muffle furnace 1.5 h of calcining to get graphene
Gas-diffusion electrode.
Embodiment 2:
A kind of preparation method of graphene gas-diffusion electrode, includes the following steps:
Step (1): by crystalline flake graphite, NaNO3It is reacted in ice-water bath with the concentrated sulfuric acid in the ratio of 3.0 g: 2g: 160 mL
1 h, then weigh 9.0437 g KMnO4In being slowly added to beaker in 3 h dropwise, 2 h are reacted;
Step (2): removing ice-water bath, is warming up to 40 DEG C or so, continues to be stirred to react 1.5 h.It is slowly added to 160 mL steaming
Distilled water is heated to boiling, and is stirred to react 1 h;
Step (3): the resulting mixed solution of step 2 is placed into a period of time, in 48-52 DEG C plus 30 mL 30% of H2O2,
175 mL distilled water are added, react 3 h, cooled and filtered.With mass fraction be 30% salt acid elution to sulfate radical-free until,
It is washed with distilled water to PH=7 again.Filter residue is dried in vacuo in 40 DEG C, and graphene oxide is made;
Step (4): weighing 100.0 mg ultrasound in 100 mL aqueous solutions for the resulting graphene oxide of step 3, until
Obtain the stable dispersions almost without obvious particle.The ammonium hydroxide that mass fraction is 28% is taken to adjust the pH to 10 of dispersion liquid;
Step (5): by the resulting solution of step 4 in 4000 rmin-1It is unstripped that 3 min of lower centrifugation remove minute quantity
Graphite oxide is added 0.2mL hydrazine hydrate into the graphene oxide dispersion after centrifugation and obtains graphite in 90 DEG C of 2 h of reaction
Alkene dispersion liquid;
Step (6): it takes 0.8 g graphite and 160 mL, 3% alcohol mixture in room temperature 10 min of ultrasound, adds obtained by step 5
10 mL of graphene dispersing solution and 0.2 g polytetrafluoroethylene (PTFE) room temperature 15 min of ultrasound, at 80 DEG C of water-bath constant temperature plus
Heat to paste takes out;
Step (7): nickel screen two sides are uniformly attached to after the resulting pasty mixture of step 6 is slightly cooling, place one section
After time mushy freezing, cold pressing 3 min molding (with a thickness of 0.5mm), in 300 DEG C of Muffle furnace 1.5 h of calcining to get graphene
Gas-diffusion electrode.
Above-described embodiment 2 is most preferred embodiment.
The resulting electrode of above-mentioned most preferred embodiment is tested in electricity-Fenton-like system, sewage used is rhodamine B
Dye wastewater.
Before use, electrode impregnates 24 h in acetone, to remove the surface-active in its ethyl alcohol remained on surface and PTFE
Substance finally with deionized water repeated flushing and is dried.Then accessing in electricity-Fenton-like system according to the method for conventional electrodes makes
With.
Test uses rhodamine B dye wastewater, and configured solution is moved 50 mL and enters Fe in beaker2+Concentration is
0.33 mol/L, using titanium plate as anode, self-control graphene gas-diffusion electrode is that cathode carries out degradation experiment, anode and cathode significant surface
Product is 0.7 cm2(long 1cm wide 0.7cm).Rhodamine B concentration is 10 mg/L, and processing volume is 50 mL, reaction time 60
Min, current density are 20 mA/cm2, electrolyte (NaSO4) concentration be 0.05 mol/L, 1 cm of electrode spacing, initial pH=3.0,
Whole process aeration.Gas-diffusion electrode obtained above (GDE) degradation efficiency is measured in electricity-Fenton-like system.As a result table
Bright, under the same terms, it is traditional carbon electrode that self-control gas-diffusion electrode, which has reached 90% in 60 min to the removal rate of rhodamine B,
(CP) 1.5 times.
Claims (3)
1. a kind of preparation method of graphene gas-diffusion electrode, includes the following steps:
Step (1): by crystalline flake graphite, NaNO31 h is reacted in ice-water bath in the ratio of 3.0 g: 2g: 160 mL with the concentrated sulfuric acid,
9.0437 g KMnO are weighed again4In being repeatedly slowly added to beaker in 3 h in batches, 2h is reacted；
Step (2): removing ice-water bath, is warming up to 40 DEG C or so, continues to be stirred to react 1.5 h；
160 mL distilled water are slowly added to, are heated to boiling, are stirred to react 1 h；
Step (3): the resulting mixed solution of step (2) is placed into a period of time, in 48-52 DEG C plus 30 mL 30% of H2O2, add
Enter 175 mL distilled water, reacts 3 h, cooled and filtered；
With mass fraction be 30% salt acid elution to sulfate radical-free until, then be washed with distilled water to pH=7；
Filter residue is dried in vacuo in 40 DEG C, and graphene oxide is made；
Step (4): it is ultrasonic in 100 mL aqueous solutions that step (3) resulting graphene oxide is weighed into 100.0 mg, until obtaining
To the stable dispersions almost without obvious particle；
The ammonium hydroxide that mass fraction is 28% is taken to adjust the pH to 10 of dispersion liquid；
Step (5): by step (4) resulting solution in 4000 rmin-13 min of lower centrifugation remove the unstripped oxygen of minute quantity
0.2 mL hydrazine hydrate is added into the graphene oxide dispersion after centrifugation for graphite, in 90 DEG C of 2 h of reaction, obtains graphene
Dispersion liquid；
Step (6): it takes the mixture of 3% ethyl alcohol of 0.8 g graphite and 160 mL in room temperature 10 min of ultrasound, adds obtained by step (5)
10 mL of graphene dispersing solution and 0.2 g polytetrafluoroethylene (PTFE) room temperature 15 min of ultrasound, at 80 DEG C of water-bath constant temperature plus
Heat to paste takes out；
Step (7): nickel screen two sides are uniformly attached to after step (6) resulting pasty mixture is slightly cooling, when placing one section
Between after mushy freezing, cold pressing 3 min molding, molding thickness 0.5mm, in 300 DEG C of Muffle furnace 1.5 h of calcining to get graphene
Gas-diffusion electrode.
2. application of the graphene gas-diffusion electrode that preparation method obtains according to claim 1 in electricity-Fenton-like system.
3. use of the graphene gas-diffusion electrode that preparation method obtains according to claim 1 in electricity-Fenton-like system
Method, it is characterised in that: before use, electrode impregnates 24 h in acetone, to remove in its ethyl alcohol remained on surface and PTFE
Surface reactive material finally with deionized water repeated flushing and is dried, and is accessed and is used according to the method for conventional electrodes.
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| CN106744828A (en) * | 2016-11-23 | 2017-05-31 | 西安工业大学 | A kind of preparation method of Novel electro-Fenton cathode material and application |
| CN106957093A (en) * | 2017-04-07 | 2017-07-18 | 西安工业大学 | A kind of preparation method of Fe skeletons graphene gas-diffusion electrode |
| CN111717966B (en) * | 2019-03-20 | 2022-06-17 | 中国石油化工股份有限公司 | Sulfate reducing bacteria electro-filtration sterilization device, graphene nanofiber non-woven fabric and preparation method of graphene nanofiber non-woven fabric |
| CN110818033A (en) * | 2019-11-20 | 2020-02-21 | 德蓝水技术股份有限公司 | Preparation method and application of graphene gas diffusion electrode in electro-Fenton system |
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