CN106957093A - A kind of preparation method of Fe skeletons graphene gas-diffusion electrode - Google Patents
A kind of preparation method of Fe skeletons graphene gas-diffusion electrode Download PDFInfo
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- 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
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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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Abstract
The present invention relates to a kind of preparation method of Fe skeletons graphene gas-diffusion electrode, belong to gas-diffusion electrode preparing technical field.Its preparation process is as follows:Powdered Activated Carbon, deionized water and absolute ethyl alcohol are mixed, and by NH4HCO3Incorporation wherein, then by PTFE emulsion is added after said mixture, sonic oscillation, and placement to the mixture is in thick-pasty and is attached in iron net, and gas-diffusion electrode is pressed on hydraulic press.Fe skeleton graphene gas-diffusion electrodes prepared by the present invention have good electric conductivity, it is provided simultaneously with excellent electric Fenton catalytic activity, it is applied to not only have good electrocatalysis characteristic in electric Fenton-like system as cathode material, and electro-Fenton reaction has been widened to pH value range, it is to avoid additional Fe2+Realize Fe simultaneously2+Recycling, it is to avoid the generation of iron cement, so that oxidation efficiency is effectively raised, while reducing cost again.The present invention is simple to operate, with low cost, is a kind of efficient, new technology of energy-conservation.
Description
Technical field
The present invention relates to a kind of preparation method of Fe skeletons-graphene gas-diffusion electrode, belong to gas-diffusion electrode
Technical field.
Background technology
For exist now organic waste water pollutant difficult degradation the problem of, high-level oxidation technology is continued to develop, electricity-
Fenton process as high-level oxidation technology one kind, due to the features such as simple to operate, oxidability is strong, degradation efficiency is high by people
Extensive concern.But current electricity-treating organic waste water by Fenton method be only suitable for pH scopes be 2-4 in the range of effect compared with
It is good, but iron ion easily produces precipitation and loses catalytic action under near-neutral sulfite deinking, treatment effect is deteriorated.In order to realize
Fe2+Electricity-Fenton's reaction is reused and widened to pH value application, ferrous metal thing is fixed on electrode, catalysis is produced
OH degraded water pollutants turn into the development trend of electricity-Fenton technology.
The content of the invention
It is an object of the invention to for it is set forth above the problem of there is provided a kind of graphene gas using iron skeleton as substrate
Diffusion electrode, organic wastewater is handled using it higher than the performance and degradation effect of other electrodes.
To realize the purpose of the present invention, implementation process of the invention is as follows:
A kind of preparation method of Fe skeletons-graphene gas-diffusion electrode, comprises the steps successively:
Step (1):Powdered Activated Carbon, deionized water and absolute ethyl alcohol are mixed in 1g: 100mL: 10mL ratio, and will
0.05g pore creating materials NH4HCO3Incorporation wherein, then is sufficiently stirred for being allowed to uniform.
Step (2):Ratio by the PTFE emulsion of step 1 gained mixed liquor and mass fraction 10% in mass ratio for 80: 1
It is sufficiently mixed, then it is well mixed through supersonic oscillations.
Step (3):Mixed solution obtained by step 2 is placed into a period of time, will when the mixture is in sticky pasty state
It is attached in a length of 1cm, a width of 0.7cm iron net, and is pressed on hydraulic press the gas diffusion electricity that thickness is 0.6mm
Pole.
Powdered Activated Carbon need to be pre-processed as follows by pretreatment in step (1):1g graphite powders are put into beaker, added
Distilled water boils 1h, removes after upper suspension, through vavuum pump suction filtration, the graphite powder after suction filtration is placed in baking oven at 106 DEG C
6h is dried, is fitted into standby in polybag.
Iron net need to be by pretreatment in step (3), and process is as follows:Iron net after cutting is placed in absolute ethyl alcohol and soaked
48h is used to remove the greasy dirt and impurity on iron net surface, after immersion, with deionized water rinsing at least three times, is placed in 105 DEG C dry
12h is dried in dry case, dried iron net is put into standby in polybag.
Before use, electrode need to soak 24h in fresh acetone, the surface in ethanol and PTFE to remove its remained on surface
Active material, is finally rinsed and dried repeatedly with deionized water.
Using above-mentioned technical proposal, the application of Fe skeletons-graphene gas-diffusion electrode of preparation, the electrode is used as negative electrode
Materials application is degraded in electricity-Fenton-like system to organic wastewater.
This experiment simulates degrading waste water using rhodamine B, and the solution configured is moved into 50mL beakers, using titanium plate as sun
Pole, self-control Fe skeletons-graphene gas-diffusion electrode is that negative electrode carries out degradation experiment, and anode and cathode effective area is 0.7cm2
(the long wide 0.7cm of 1cm).Rhodamine B concentration is 10mg/L, and processing volume is 50mL, reaction time 60min, and current density is
20mA/cm2, electrolyte (NaSO4) concentration be 0.05mol/L, electrode spacing 1cm, initial pH=3.0, whole process aeration.
Compared with prior art, it is an advantage of the invention that:
First, it is prevented effectively from the generation of iron cement:Fe skeletons-graphene gas-diffusion electrode prepared by the present invention, due to Fe bones
Frame-graphene gas-diffusion electrode has loose structure, therefore has to organic dyestuff stronger absorption property;And Fe skeletons-stone
Black alkene gas-diffusion electrode thickness is smaller, is conducive to transmission of the gas by microcellular structure from solution to electrode surface.Fe skeletons-
Graphene gas-diffusion electrode can avoid additional Fe2+, while iron cement can be prevented effectively from electricity-Fenton-like system as negative electrode
Produce.
2nd, the pH scope of applications are wide:This product is applied in electricity-Fenton-like system, is not only protected in the range of pH scopes are 2-4
High degradation rate is held, while there is higher degradation rate in pH neutral, more than 89.53% is can reach, therefore can be met pair
The degraded of all kinds of organic wastewaters.
Brief description of the drawings:
Fig. 1 is Fe skeletons-graphene gas-diffusion electrode and gas-diffusion electrode and nickel screen graphene gas in embodiment one
The linear scan curve map of body diffusion electrode;
Fig. 2 is Fe skeletons-graphene gas-diffusion electrode and gas-diffusion electrode and nickel screen graphene gas in embodiment one
The cyclic voltammetry curve figure of body diffusion electrode;
Fig. 3 is Fe skeletons-graphene gas-diffusion electrode and gas-diffusion electrode and nickel screen graphene gas in embodiment two
The degraded figure of body diffusion electrode and carbon plate in electricity-Fenton-like system to rhodamine B;
Fig. 4 be embodiment two in Fe skeletons-graphene gas-diffusion electrode under the wide pH value of electricity-Fenton-like system to rhodamine
B degraded figure.
Embodiment is as follows:
Graphene gas-diffusion electrode (GDE) has loose structure, and thickness of electrode is smaller, is conducive to gas to pass through micropore
Transmission of the structure from solution to electrode surface.Graphene gas-diffusion electrode substrate of the present invention is iron skeleton, by iron internalization to electricity
It is extremely internal, applied to can both improve its oxidation efficiency in electricity-Fenton-like system, cost is reduced again, while can overcome
Fe2+It can not reuse and the problems such as poor processing effect, can be met to having under electricity-treating organic waste water by Fenton method neutrallty condition
The degraded of machine thing waste water.
Embodiment one:
A kind of preparation of Fe skeletons-graphene gas-diffusion electrode:
Powdered Activated Carbon, deionized water and absolute ethyl alcohol are mixed in 1g: 100mL: 10mL ratio, and 0.05g is made
Hole agent NH4HCO3Incorporation wherein, then is sufficiently stirred for being allowed to uniform, then by gained mixed liquor and PTFE that mass fraction is 10%
Emulsion is sufficiently mixed for 80: 1 ratio in mass ratio, then is well mixed it through supersonic oscillations.A period of time is placed, this is treated
Mixture is attached in a length of 1cm, a width of 0.7cm iron net when being in sticky pasty state, and is pressed on hydraulic press thickness
Spend the gas-diffusion electrode for 0.6mm.Before use, electrode need to soak 24h in fresh acetone, to remove the second of its remained on surface
Surface reactive material in alcohol and PTFE, is finally rinsed and dried repeatedly with deionized water.
A Fe skeletons-graphene gas-diffusion electrode prepared is with being not added with Graphene electrodes and nickel screen by the following examples
Electrode is compared, and has carried out the experiment of electrochemical gaging, compares LSV the and CV curves of three, description of test is in iron net electrode
On can not only occur reversible redox reaction, and be conducive to the degraded to organic wastewater:
As shown in figure 1, iron net electrode, nickel screen electrode and be not added with Graphene electrodes -1V or so be in crest the reason for be by
In addition voltage change speed quickly, when reach deoxidation agent decomposition voltage when, the material is reduced rapidly on electrode, production
Give birth to very big electric current.Because oxidant is reduced rapidly on electrode, its concentration near electrode is drastically reduced, thickness is spread
Degree increase, and the oxidant in solution main body has little time to be diffused into electrode, thus electric current declines rapidly, when electrode reaction speed with
When diffusion velocity reaches balance, electric current would not change again, form crest electric current.And three compares iron net electrode and nickel screen electrode
Because being reversible electrode there is crest electric current, but it is the electrode for being not added with graphene for irreversible electrode, due to electrode
Reaction speed is slow, and in quick scanning, electrode reaction speed does not catch up with oxidation rate, and volt-ampere curve will occur without electric current.
As shown in Fig. 2 iron net electrode two oxidation peaks occurs in -0.75V and -0.85V or so, it is not added with Graphene electrodes and does not have
Occur oxidation peak and illustrate that its redox property is bad.There is reduction peak, iron net in -1.2V or so in negative sense scanning nickel screen electrode
There is reduction peak in -0.85V or so in electrode, and is not added with Graphene electrodes also without there is peak value.It is indicated above that iron net electrode
On can occur redox reaction because curve closure product existence is more stable.Because there is multigroup oxidation in it
Peak, so the redox property in rhodamine B is preferably, degradation effect is best.
Embodiment two:
This experiment simulates degrading waste water using rhodamine B, and the solution configured is moved into 50mL beakers, using titanium plate as sun
Pole, respectively with nickel screen graphene gas-diffusion electrode, be not added with product made from the gas-diffusion electrode and the present embodiment of graphene
Degradation experiment is carried out for negative electrode, anode and cathode effective area is 0.7cm2(the long wide 0.7cm of 1cm).Rhodamine B concentration is 10mg/
L, processing volume is 50mL, and reaction time 60min, current density is 20mA/cm2, electrolyte (NaSO4) concentration be 0.05mol/
L, electrode spacing 1cm, initial pH=3.0, whole process aeration.Gas-diffusion electrode degradation efficiency obtained above is measured.
As a result show:Self-control Fe skeletons-graphene gas-diffusion electrode does negative electrode, degradation efficiency highest.
Below by way of product made from nickel screen graphene gas-diffusion electrode, gas-diffusion electrode, carbon plate and embodiment one
Degradation experiment is carried out, compares four degradation efficiency:As shown in figure 3, during rhodamine B degradation, loading the negative electrode of graphene
The degradation efficiency of material degradation rhodamine B is higher than the cathode material and carbon plate of unsupported graphene, so as to embody graphene gas
The superiority of diffusion electrode;In the iron net electrode and nickel screen electrode that have loaded graphene simultaneously, the final degradation effect of iron net is more
It is good.
As shown in figure 4, product made from embodiment one is used as cathode material rhodamine B degradation, in pH=7, degradation rate
Still have 89.53%, illustrate Fe skeletons-graphene gas-diffusion electrode applied to degradable organic pollutant in electricity-Fenton-like system not
The good degrading effect only in pH=3, still there is higher degradation rate in neutral conditions.
, need not be again in degradation experiment because Fe skeletons-graphene gas-diffusion electrode is using iron net as substrate in this experiment
Additional iron ion, while on electricity-Fenton-like system negative electrode, Fe3+Electronics can be obtained and be converted into Fe2+, continue to participate in after electricity-Fenton
Continuous reaction, therefore compared to nickel screen graphene gas-diffusion electrode, Fe skeletons-graphene gas-diffusion electrode as negative electrode electricity-
The generation of iron cement can be prevented effectively from Fenton-like system.
Claims (4)
1. a kind of preparation method of Fe skeletons-graphene gas-diffusion electrode, it is characterised in that:The preparation method includes successively
Following step:
Step (1):Powdered Activated Carbon, deionized water and absolute ethyl alcohol are mixed in 1g: 100mL: 10mL ratio, and will
0.05g pore creating materials NH4HCO3Incorporation wherein, then is sufficiently stirred for being allowed to uniform.
Step (2):The PTFE emulsion of step 1 gained mixed liquor and mass fraction 10% is abundant in mass ratio for 80: 1 ratio
Mixing, then it is well mixed it through supersonic oscillations.
Step (3):Mixed solution obtained by step 2 is placed into a period of time, it is when the mixture is in sticky pasty state that its is attached
On a length of 1cm, a width of 0.7cm iron net, and be pressed on hydraulic press the gas-diffusion electrode that thickness is 0.6mm.
2. a kind of preparation method of Fe skeletons-graphene gas-diffusion electrode according to claim 1, it is characterised in that:
Powdered Activated Carbon need to be pre-processed as follows by pretreatment in step (1):1g graphite powders are put into beaker, distillation is added
Water boils 1h, removes after upper suspension, through vavuum pump suction filtration, the graphite powder after suction filtration is placed in baking oven at 106 DEG C and dried
6h, is fitted into standby in polybag.
3. a kind of preparation method of Fe skeletons-graphene gas-diffusion electrode according to claim 1, it is characterised in that:
Iron net need to be by pretreatment in step (3), and process is as follows:Iron net after cutting is placed in absolute ethyl alcohol and soaks 48h use
In the greasy dirt and impurity that remove iron net surface, after immersion, with deionized water rinsing at least three times, 105 DEG C of drying box is placed in
Middle dry 12h, dried iron net is put into standby in polybag.
4. Fe skeletons-graphene gas-diffusion electrode as claimed in claim 1 is applied in electricity-Fenton-like system as cathode material
In organic wastewater is degraded.
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
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CN109850896A (en) * | 2017-11-30 | 2019-06-07 | 中南民族大学 | A kind of preparation method and application of primary Eichhornia crassipes biomass carbon porous electrode material |
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CN105836855A (en) * | 2016-06-13 | 2016-08-10 | 西安工业大学 | Preparation method and application of graphene gas diffusion electrode |
CN106104877A (en) * | 2014-03-28 | 2016-11-09 | 东丽株式会社 | Gas-diffusion electrode and manufacture method thereof |
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2017
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WO2002026636A1 (en) * | 2000-09-29 | 2002-04-04 | Aqua Butzke Gmbh | Device for electrolytic water disinfection without cathodic hydrogen evolution |
CN101531411A (en) * | 2009-04-10 | 2009-09-16 | 同济大学 | Method for electrochemically disinfecting gas diffusion electrode system |
CN106104877A (en) * | 2014-03-28 | 2016-11-09 | 东丽株式会社 | Gas-diffusion electrode and manufacture method thereof |
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CN109850896A (en) * | 2017-11-30 | 2019-06-07 | 中南民族大学 | A kind of preparation method and application of primary Eichhornia crassipes biomass carbon porous electrode material |
CN109850896B (en) * | 2017-11-30 | 2020-08-11 | 中南民族大学 | Preparation method and application of native eichhornia crassipes biomass carbon porous electrode material |
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Application publication date: 20170718 |