CN105836855A - Preparation method and application of graphene gas diffusion electrode - Google Patents
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 invention relates to the technical field of the preparation of an electrode material, in particular to a preparation method and application of a graphene gas diffusion electrode. The preparation method comprises the following steps: mixing flake graphite, NaNO3 and concentrated sulfuric acid in an ice bath to obtain a mixture, enabling the mixture to slowly react with KMnO4, adding 30 percent of H2O2 to react sufficiently, filtering, washing until the solution is neutral, and drying; ultrasonically dispersing a product in an aqueous solution to obtain a dispersion solution, adjusting the pH, centrifuging, collecting an upper layer of stable solution, adding an appropriate amount of hydrazine hydrate to obtain a graphene dispersion solution; uniformly mixing the dispersion solution with graphite powder, ethanol and PTFE emulsion; and keetping constant temperature in a water bath until the mixture is in thick paste shape, attaching the mixture onto a stainless steel net, and pressing to obtain the graphene gas diffusion electrode. The graphene gas diffusion electrode is higher in oxidation capacity in an electricity-Fenton system and can be used for treating various waste water containing organic pollutants.
Description
Technical field
The present invention relates to technical field of sewage, be specifically related to preparation method and the using method thereof of a kind of Graphene gas-diffusion electrode.
Background technology
Electricity-Fenton process is as the one of high-level oxidation technology, and because of it, degraded is thorough, efficiency is high, simple to operate, time consumption and energy consumption is few, by the common concern of people in field of Environment Protection, is widely used in the process containing organic pollutant wastewater.In order to improve the catalysis activity to two electronic reduction reactions of dissolved oxygen of negative electrode in electricity-Fenton-like system, promote the further development of electricity Fenton oxidation technology, the preparation of electrode material and be selected to the new focus of this area research.Traditional cathode material used by electricity-Fenton-like system is mainly graphite, activated carbon or NACF etc., and the catalysis activity of such electrode is not high enough, and current efficiency is relatively low, and therefore the application of electricity-Fenton process is by certain restriction.
Summary of the invention
It is an object of the invention to provide preparation method and the application of a kind of Graphene gas-diffusion electrode, to improve catalysis activity and the current efficiency of electrode in electricity-Fenton-like system.
To achieve these goals, present invention provide the technical scheme that the preparation method of a kind of Graphene gas-diffusion electrode, comprise the steps:
Step (1): by crystalline flake graphite, NaNO3In ice-water bath, react 1 h with concentrated sulphuric acid in the ratio of 3.0 g: 1.5 ~ 2g: 160 mL, then weigh 9.0437 g KMnO4In 3 h, dropwise it is slowly added to beaker, reacts 2 h；
Step (2): remove ice-water bath, is warmed up to about 40 DEG C, continues stirring reaction 1.5 h；It is slowly added to 160 mL distilled water, is heated to boiling, stirring reaction 1 h；
Step (3): the mixed solution of step 2 gained is placed a period of time, adds 30 mL in 48-52 DEG C
The H of 30%2O2, add 175 mL distilled water, react 3 h, cooled and filtered；With the salt acid elution that mass fraction is 30% to sulfate radical-free, then being washed with distilled water to PH=7, filtering residue, in 40 DEG C of vacuum drying, prepares graphene oxide；
Step (4): the graphene oxide of step 3 gained weighs 100.0 mg ultrasonic in 100 mL aqueous solutions, until obtaining the stable dispersions almost without obvious granule；Take the pH to 10 of the ammonia regulation dispersion liquid that mass fraction is 28%；
Step (5): by the solution of step 4 gained at 4000 r min-1It is centrifuged down 3 min and removes the graphite oxide that very small amount is unstripped, the graphene oxide dispersion after centrifugal adds 0.2mL hydrazine hydrate, reacts 2 h at 90 DEG C, obtain graphene dispersing solution;
Step (6): take 0.8 g graphite and 160 mL
3% alcohol mixture, in ultrasonic 10 min of room temperature, adds graphene dispersing solution 10 ~ 30 mL and 0.2 ultrasonic 15 min of g polytetrafluoroethylene (PTFE) room temperature of step 5 gained, is heated to pasty state water-bath constant temperature 80 DEG C and takes out；
Step (7): be uniformly attached to nickel screen both sides after the pasty mixture of step 6 gained somewhat cools down, after placing a period of time mushy freezing, cold pressing 3 min molding (thickness is 0.5-0.7 mm), calcine 1.5 h in Muffle furnace 300 DEG C, obtain Graphene gas-diffusion electrode.
The Graphene gas-diffusion electrode that above-mentioned preparation method obtains application in electricity-Fenton-like system.
The Graphene gas-diffusion electrode that above-mentioned preparation method obtains using method in electricity-Fenton-like system, before using, electrode soaks 24 h in acetone, to remove the surfactant in the ethanol of its remained on surface and PTFE, finally repeatedly rinse with deionized water and dry, accessing according to the method for conventional electrodes and use.
Compared with prior art, the invention have the advantage that
1, it is a kind of gas-diffusion electrode adulterated by Graphene made by the present invention, compared to common gases diffusion electrode, the catalysis characteristics of Graphene itself and high-specific surface area are that Graphene gas-diffusion electrode provides more excellent reaction condition and place, thus show higher catalysis activity and current efficiency in electricity-Fenton-like system；
2, in calcination process, polytetrafluoro volume reduces, and the porosity of electrode own increases, so that this electrode increases with effective contact area of solution during electricity-Fenton's reaction, promotes the raw H of electricity2O2Yield increases, and is effectively increased the formation efficiency of hydroxyl radical free radical, strengthens the oxidability of system；
3, applied widely: to can be used in all kinds of process containing organic pollutant wastewater.
Accompanying drawing explanation
Fig. 1 is the Graphene gas-diffusion electrode material object photo prepared by embodiment 2；
Fig. 2 is the scanning electron microscope (SEM) of the Graphene gas-diffusion electrode prepared by embodiment 2；
Fig. 3 be embodiment 2 Different electrodes in electricity-Fenton-like system to rhodamine B degradation efficiency.(CP: conventional carbon electrode；DGE: Graphene gas-diffusion electrode).
Detailed description of the invention
Below in conjunction with drawings and Examples, the present invention is described in detail.
Embodiment 1:
The preparation method of a kind of Graphene gas-diffusion electrode, comprises the steps:
Step (1): by crystalline flake graphite, NaNO3In ice-water bath, react 1 h with concentrated sulphuric acid in the ratio of 3.0 g: 1.5 g: 160 mL, then weigh 9.0437 g KMnO4In 3 h, dropwise it is slowly added to beaker, reacts 2 h;
Step (2): remove ice-water bath, is warmed up to about 40 DEG C, continues stirring reaction 1.5 h.It is slowly added to 160 mL distilled water, is heated to boiling, stirring reaction 1 h;
Step (3): the mixed solution of step 2 gained is placed a period of time, adds 30 mL in 48-52 DEG C
The H of 30%2O2, add 175 mL distilled water, react 3 h, cooled and filtered.With the salt acid elution that mass fraction is 30% to sulfate radical-free, then it is washed with distilled water to PH=7.Filtering residue, in 40 DEG C of vacuum drying, prepares graphene oxide;
Step (4): the graphene oxide of step 3 gained weighs 100.0 mg ultrasonic in 100 mL aqueous solutions, until obtaining the stable dispersions almost without obvious granule.Take the pH to 10 of the ammonia regulation dispersion liquid that mass fraction is 28%;
Step (5): by the solution of step 4 gained at 4000 r min-1It is centrifuged down 3 min and removes the graphite oxide that very small amount is unstripped, the graphene oxide dispersion after centrifugal adds 0.2mL hydrazine hydrate, reacts 2 h at 90 DEG C, obtain graphene dispersing solution;
Step (6): take 0.8 g graphite and 160 mL
3% alcohol mixture, in ultrasonic 10 min of room temperature, adds graphene dispersing solution 30 mL and 0.2 ultrasonic 15 min of g polytetrafluoroethylene (PTFE) room temperature of step 5 gained, is heated to pasty state water-bath constant temperature 80 DEG C and takes out;
Step (7): be uniformly attached to nickel screen both sides after the pasty mixture of step 6 gained somewhat cools down, after placing a period of time mushy freezing, cold pressing 3 min molding (thickness is 0.7 mm), calcine 1.5 h in Muffle furnace 300 DEG C, obtain Graphene gas-diffusion electrode.
Embodiment 2:
The preparation method of a kind of Graphene gas-diffusion electrode, comprises the steps:
Step (1): by crystalline flake graphite, NaNO3In ice-water bath, react 1 h with concentrated sulphuric acid in the ratio of 3.0 g: 2g: 160 mL, then weigh 9.0437 g KMnO4In 3 h, dropwise it is slowly added to beaker, reacts 2 h;
Step (2): remove ice-water bath, is warmed up to about 40 DEG C, continues stirring reaction 1.5 h.It is slowly added to 160 mL distilled water, is heated to boiling, stirring reaction 1 h;
Step (3): the mixed solution of step 2 gained is placed a period of time, adds 30 mL in 48-52 DEG C
The H of 30%2O2, add 175 mL distilled water, react 3 h, cooled and filtered.With the salt acid elution that mass fraction is 30% to sulfate radical-free, then it is washed with distilled water to PH=7.Filtering residue, in 40 DEG C of vacuum drying, prepares graphene oxide;
Step (4): the graphene oxide of step 3 gained weighs 100.0 mg ultrasonic in 100 mL aqueous solutions, until obtaining the stable dispersions almost without obvious granule.Take the pH to 10 of the ammonia regulation dispersion liquid that mass fraction is 28%;
Step (5): by the solution of step 4 gained at 4000 r min-1It is centrifuged down 3 min and removes the graphite oxide that very small amount is unstripped, the graphene oxide dispersion after centrifugal adds 0.2mL hydrazine hydrate, reacts 2 h at 90 DEG C, obtain graphene dispersing solution;
Step (6): take 0.8 g graphite and 160 mL
3% alcohol mixture, in ultrasonic 10 min of room temperature, adds graphene dispersing solution 10 mL and 0.2 ultrasonic 15 min of g polytetrafluoroethylene (PTFE) room temperature of step 5 gained, is heated to pasty state water-bath constant temperature 80 DEG C and takes out;
Step (7): be uniformly attached to nickel screen both sides after the pasty mixture of step 6 gained somewhat cools down, after placing a period of time mushy freezing, cold pressing 3 min molding (thickness is 0.5mm), calcine 1.5 h in Muffle furnace 300 DEG C, obtain Graphene gas-diffusion electrode.
Above-described embodiment 2 is most preferred embodiment.
Being tested in electricity-Fenton-like system by the electrode of above-mentioned most preferred embodiment gained, sewage used is rhodamine B dye wastewater.
Before using, electrode soaks 24 h in acetone, to remove the surfactant in the ethanol of its remained on surface and PTFE, finally repeatedly rinses with deionized water and dries.Use then according to the method for conventional electrodes accesses in electricity-Fenton-like system.
Test uses rhodamine B dye wastewater, the solution configured is moved 50 mL and enters Fe in beaker2+Concentration is 0.33 mol/L, and with titanium plate as anode, self-control Graphene gas-diffusion electrode is that negative electrode carries out degradation experiment, and anode and cathode effective area is 0.7 cm2(long 1cm width 0.7cm).Rhodamine B concentration is 10 mg/L, and processing volume is 50 mL, and response time 60 min, electric current density is 20 mA/cm2, electrolyte (NaSO4) concentration is 0.05 mol/L, electrode spacing 1 cm, initial pH=3.0, omnidistance aeration.Above-mentioned prepared gas-diffusion electrode (GDE) degradation efficiency is measured by electricity Fenton-like system.Result shows, under the same terms, self-control gas-diffusion electrode has reached 90% to the clearance of rhodamine B at 60 min, is 1.5 times of conventional carbon electrode (CP).
Claims (3)
1. the preparation method of a Graphene gas-diffusion electrode, it is characterised in that comprise the steps:
Step (1): by crystalline flake graphite, NaNO3In ice-water bath, react 1 h with concentrated sulphuric acid in the ratio of 3.0 g: 1.5 ~ 2g: 160 mL, then weigh 9.0437 g KMnO4In 3 h, dropwise it is slowly added to beaker, reacts 2 h；
Step (2): remove ice-water bath, is warmed up to about 40 DEG C, continues stirring reaction 1.5 h；It is slowly added to 160 mL distilled water, is heated to boiling, stirring reaction 1 h；
Step (3): the mixed solution of step 2 gained is placed a period of time, adds the H of 30 mL 30% in 48-52 DEG C2O2, add 175 mL distilled water, react 3 h, cooled and filtered；With the salt acid elution that mass fraction is 30% to sulfate radical-free, then being washed with distilled water to PH=7, filtering residue, in 40 DEG C of vacuum drying, prepares graphene oxide；
Step (4): the graphene oxide of step 3 gained weighs 100.0 mg ultrasonic in 100 mL aqueous solutions, until obtaining the stable dispersions almost without obvious granule；Take the pH to 10 of the ammonia regulation dispersion liquid that mass fraction is 28%；
Step (5): by the solution of step 4 gained at 4000 r min-1It is centrifuged down 3 min and removes the graphite oxide that very small amount is unstripped, the graphene oxide dispersion after centrifugal adds 0.2mL hydrazine hydrate, reacts 2 h at 90 DEG C, obtain graphene dispersing solution；
Step (6): take 0.8 g graphite and 160 mL 3% alcohol mixtures in ultrasonic 10 min of room temperature, add graphene dispersing solution 10 ~ 30 mL and 0.2 ultrasonic 15 min of g polytetrafluoroethylene (PTFE) room temperature of step 5 gained, be heated to pasty state water-bath constant temperature 80 DEG C and take out；
Step (7): be uniformly attached to nickel screen both sides after the pasty mixture of step 6 gained somewhat cools down, after placing a period of time mushy freezing, 3 min molding of colding pressing (thickness is 0.5-
0.7 mm), calcine 1.5 h in Muffle furnace 300 DEG C, obtain Graphene gas-diffusion electrode.
2. the Graphene gas-diffusion electrode obtained according to the above-mentioned preparation method application in electricity-Fenton-like system.
3. the Graphene gas-diffusion electrode obtained according to the above-mentioned preparation method using method in electricity-Fenton-like system, it is characterized in that: before use, electrode soaks 24 h in acetone, to remove the surfactant in the ethanol of its remained on surface and PTFE, finally repeatedly rinse with deionized water and dry, accessing according to the method for conventional electrodes and use.
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Cited By (4)
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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 |
| 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 |
| CN111717966A (en) * | 2019-03-20 | 2020-09-29 | 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 |
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