CN110436584A - A kind of PPy/GO combination electrode material, preparation method and applications - Google Patents
A kind of PPy/GO combination electrode material, preparation method and applications 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
- C02F1/469—Treatment of water, waste water, or sewage by electrochemical methods by electrochemical separation, e.g. by electro-osmosis, electrodialysis, electrophoresis
- C02F1/4691—Capacitive deionisation
Abstract
The invention discloses a kind of PPy/GO combination electrodes, preparation method and applications, belong to capacitive deionization technical field.Preparation method of the present invention is using foam nickel base as collector, pyrrole monomer is dissolved in neopelex (SDBS) solution first, then graphene oxide dispersion is added, ultrasonic disperse and after being sufficiently stirred, PPy/GO composite deposite is generated in foamed nickel current collector by the method that a step anode electrochemical is co-deposited, cleaning, it is dry, PPy/GO combination electrode is made.The method that the present invention prepares electrode material is simple, it can operate strong with repeatability, suitable for batch production, electrode material more adsorption sites are assigned while the synergistic effect of GO and PPy are obviously improved electrode material electric conductivity, further improve the capacitive property and adsorption desorption performance of electrode material.
Description
Technical field
The invention belongs to capacitive deionization technical fields, more particularly to a kind of PPy/GO combination electrode material, preparation
Method and its application.
Background technique
In recent years, capacitive deionization technology as processing energy crisis and problem of environmental pollution a kind of advanced technology by
The concern of researcher is arrived.About electrode material, conducting polymer is as capacitive deionization technology electrode material, at present
Become the hot spot of research.Conducting polymer not only has good electric conductivity, but also shows excellent ion-exchange performance.
Polypyrrole (PPy) is used as a kind of typical conducting polymer, with specific capacitance is high, conductivity is high, at low cost, chemical stability is good
The advantages that, but its cyclical stability in charge and discharge process is preferable.In terms of the preparation of electrode, main compression forming at present and viscous
Knot forming method prepares electrode material, and that there are preparation processes is complicated for the method, electrode moulding is difficult, repeatability can be bad etc. lacks
It falls into.
Summary of the invention
In order to overcome the disadvantages of the above prior art, the object of the present invention is to provide a kind of electrochemical depositions to prepare PPy/GO
The method of combination electrode.Because graphene oxide (GO) has good mechanical tenacity, good mechanical property, preferable heat steady
Fixed and chemical stability etc., and there are higher specific surface area (SAA) by GO, and contain a large amount of oxygen-containing groups, have it
Good hydrophilicity is simultaneously easily dispersed in aqueous solution, is easy to form composite material with other components.The bigger serface of GO
A large amount of polymerization sites can be provided for py monomer, and limit its reunion, to provide the nucleation site for depositing PPy.Therefore,
It can be used as a kind of good capacitive deionization electrode material in conjunction with the composite material of PPy and GO, and use electrochemical deposition
Method make electrode moulding condition simple and can prepare efficient uniform electrode material.
To achieve the above object, the present invention provides following schemes:
The present invention provides a kind of preparation methods of PPy/GO combination electrode, comprising the following steps:
Step 1: pyrrole monomer is added in neopelex solution and stirs evenly, obtains finely dispersed
Mixed liquor A；
Step 2: graphene oxide dispersion being added into step 1 mixed liquor A, and ultrasonic disperse to uniform state obtains
Finely dispersed mixed solution B；
Step 3: using nickel foam as anode, homalographic graphite plate is as cathode, with mixed solution B described in step 2
Make electrolyte, carries out electrochemical deposition and obtain PPy/GO complex capacitance deionization electrode material.
Further, the volume ratio of neopelex solution and pyrrole monomer is 500:7 in step 1, when stirring
Between be 20min.
Further, in step 2, graphene oxide dispersion the preparation method is as follows:
3g NaNO is added in 500mL round-bottomed flask3, 3g graphite and the dense H of 100mL2SO4, persistently stirred in ice-water bath
30min is reacted, by 9g KMnO4It is slowly added to flask with vigorous stirring, then removes ice bath, mixed solution is held at 35 DEG C
Then 100mL double distilled water is added in continuous stirring 1h, 90 DEG C of the temperature holding of mixed liquor is hereinafter, be added 80mL H2O2, until in flask
Bubble-free generates, and reaction terminates, and the color of reaction product gradually becomes glassy yellow from dark-brown, obtains mixed solution C, mixes molten
Liquid C centrifuge separation, centrifugation time 4min, revolving speed 7000r/min are added deionized water and produce gained after being separated by solid-liquid separation
Object, which is added, to be passed through in pretreated bag filter, seals upper lower sealing, then put it into the sink full of deionized water and carry out thoroughly
Analysis is examined with pH analyzer, and as pH=7, dialysis is completed, and appropriate amount of deionized water is added in the graphene oxide after dialysis and is carried out
The graphene oxide dispersion of 1g/L is configured to after freeze-drying.
Further, the volume ratio of graphene oxide dispersion and mixed liquor A is 1:1 in step 2.
Further, ultrasonic power is 200W, ultrasonic time 10min in step 2.
Further, bag filter preprocessing process are as follows: bag filter is processed as 20cm length cell, and is heated in the hot water
10min, cooling are spare.
Further, under room temperature, electrochemical deposition voltage is 3.0V, sedimentation time 25-30min, deposition process
In electrolyte is stirred.
The present invention also provides a kind of PPy/GO combination electrode materials being prepared according to the preparation method.
The present invention also provides the applications in absorption waste water of the PPy/GO combination electrode material.
Further, the waste water is the waste water containing heavy metal.
Further, the heavy metal in the waste water containing heavy metal is copper, and aluminium, zinc, nickel and lead etc. are a kind of or several
Kind.
The invention discloses following technical effects:
Electrode material prepared by the present invention includes foam nickel base and composite electrodeposition layer, and electrode material is mainly by nickel foam
Substrate, polypyrrole (PPy), graphene oxide (GO) composition.The preparation method of electrode material is using foam nickel base as afflux
Pyrrole monomer is dissolved in neopelex (SDBS) solution first, graphene oxide dispersion is then added by body, surpasses
After sound disperses and is sufficiently stirred, it is multiple that PPy/GO is generated in foamed nickel current collector by the method that a step anode electrochemical is co-deposited
Coating is closed, is cleaned, it is dry, PPy/GO complex capacitance deionization electrode material is made.The present invention prepares the method letter of electrode material
It is single, it can operate strong with repeatability, be suitable for batch production.
The present invention provides a kind of methods that electrochemical deposition prepares PPy/GO combination electrode, are made by the method for the invention
PPy/GO combination electrode electrode than pure PPy have higher capacitive property and Electro Sorb/desorption performance.Because of graphene oxide
(GO) there is good mechanical tenacity, good mechanical property, preferable thermostabilization and chemical stability etc., and GO piece exists
Higher specific surface area (SAA), and contain oxygen-containing group, it is readily dispersed in water, forms composite material with other components.
The reunion that GO big SAA can effectively disperse the PPy to be formed and limit PPy, contends with because the oxygen-containing group of GO can play
The interaction of ion and the PPy chain of formation, to provide the nucleation site for depositing PPy.Therefore, in conjunction with PPy's and GO
Composite material can be used as a kind of good CDI material.Using the method for electrochemical deposition electrode moulding is easy and makes
Standby efficiency improves.
Detailed description of the invention
It in order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, below will be to institute in embodiment
Attached drawing to be used is needed to be briefly described, it should be apparent that, the accompanying drawings in the following description is only some implementations of the invention
Example, for those of ordinary skill in the art, without creative efforts, can also obtain according to these attached drawings
Obtain other attached drawings.
Fig. 1 is the SEM figure that electrochemical deposition prepares electrode, wherein the SEM that (a) is pure PPy electrode prepared by the present invention schemes,
(b) the SEM figure of the PPy/GO combination electrode prepared for embodiment 1；
Fig. 2 is pure PPy electrode prepared by embodiment 1 and PPy/GO combination electrode Electro Sorb Cu prepared by embodiment 22+When inhale
Attached saturation curve；
Fig. 3 is PPy/GO combination electrode Electro Sorb various concentration Cu made from embodiment 22+When adsorbance change with time
Curve；
Fig. 4 is PPy/GO combination electrode Electro Sorb Cu made from embodiment 22+Adsorbance is at any time under Shi Butong clamping voltage
Change curve；
Fig. 5 is that the PPy/GO combination electrode obtained of the embodiment of the present invention 2 has carried out 5 adsorption/desorption circulation experiments；
Fig. 6 is the X ray diffracting spectrum of the GO obtained of the embodiment of the present invention 2；
Fig. 7 is electric deposition device figure of the present invention；
Fig. 8 is the PPy/GO combination electrode of the preparation of the embodiment of the present invention 2 to Ag+,Cu2+,Pb2+,Cd2+And Fe3+Five kinds of metals
The saturated extent of adsorption of ion.
Specific embodiment
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete
Site preparation description, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.It is based on
Embodiment in the present invention, it is obtained by those of ordinary skill in the art without making creative efforts every other
Embodiment shall fall within the protection scope of the present invention.
In order to make the foregoing objectives, features and advantages of the present invention clearer and more comprehensible, with reference to the accompanying drawing and specific real
Applying mode, the present invention is described in further detail.
Embodiment 1
The pure PPy electrode preparation method of the present embodiment carries out in accordance with the following steps:
Step 1: being added pyrrole monomer 2.8mL in 200mL 0.1M neopelex solution, stirs 20min,
Obtain uniform mixed solution；Neopelex solution is that 32.6g detergent alkylate sulphur is added into 1L deionized water
Acid is stirred for the neopelex solution being formed uniformly；
Step 2: nickel foam substrate being put into the mixed liquor of step 1 formation and do anode, and graphite plate does cathode, connection electricity
Source carries out electrochemical deposition, and depositing temperature is 25 DEG C, deposition voltage 3.0V, sedimentation time 25min, obtains pure PPy electrode.
Embodiment 2
The preparation method of the PPy/GO combination electrode of the present embodiment carries out in accordance with the following steps:
Step 1: being added pyrrole monomer 1.4mL in 100mL neopelex solution, stirs 20min, obtains
Uniform mixed solution；Neopelex solution is the addition 32.6g dodecyl benzene sulfonic acid into 1L deionized water, then
Stir evenly the neopelex solution to be formed；
Step 2: being added the graphene oxide dispersion that 100mL concentration is 1g/L in the mixed liquor formed again to step 1,
Mixed solution ultrasound 10min, magnetic agitation 20min are obtained into uniform mixed solution；Wherein, graphene oxide is to use to change
Into Hummers method preparation, in 500mL round-bottomed flask be added 3g NaNO3, 3g graphite and the dense H of 100mL2SO4, in ice water
30min is persistently stirred to react in bath.By 9g KMnO4It is slowly added in flask with vigorous stirring, then removes ice bath, mix
Solution persistently stirs 1h at 35 DEG C, 100mL double distilled water is then added, 90 DEG C of the temperature holding of mixed liquor is hereinafter, be added
80mL H2O2, until bubble-free generates in flask, reaction terminates.The color of reaction product gradually becomes glassy yellow from dark-brown, obtains
To mixed solution C.Mixed solution C is separated by centrifuge separation mode, centrifugation time 4min, revolving speed 7000r/min, into
Row a small amount of deionized water is added after being separated by solid-liquid separation and products therefrom is added in bag filter (bag filter pre-processes: by bag filter plus
Work is 20cm length cell, and heats 10min in the hot water, and cooling is spare), upper lower sealing is sealed, then put it into be full of and go
It dialyses in the sink of ionized water, is examined with pH analyzer, as pH=7, dialysis is completed, by the graphene oxide after dialysis
It is added after appropriate amount of deionized water is freeze-dried and prepares the graphene oxide dispersion of 1g/L；
Step 3: nickel foam substrate being put into the mixed liquor of step 2 formation and do anode, and graphite plate does cathode, connection electricity
Source carries out electrochemical deposition, and deposition voltage 3.0V, sedimentation time 25min obtain pure PPy/GO combination electrode.
Embodiment 3
The preparation method of the PPy/GO combination electrode of the present embodiment carries out in accordance with the following steps:
Step 1: being added pyrrole monomer 1.4mL in 100mL neopelex solution, stirs 20min, obtains
Uniform mixed solution；Neopelex solution is the addition 32.6g dodecyl benzene sulfonic acid into 1L deionized water, then
Stir evenly the neopelex solution to be formed；
Step 2: being added the graphene oxide dispersion that 100mL concentration is 1g/L in the mixed liquor formed again to step 1,
Mixed solution ultrasound 10min, magnetic agitation 20min are obtained into uniform mixed solution；Wherein, graphene oxide is to use to change
Into Hummers method preparation, in 500mL round-bottomed flask be added 3g NaNO3, 3g graphite and the dense H of 100mL2SO4, in ice water
30min is persistently stirred to react in bath.By 9g KMnO4It is slowly added in flask with vigorous stirring, then removes ice bath, mix
Solution persistently stirs 1h at 35 DEG C, 100mL double distilled water is then added, 90 DEG C of the temperature holding of mixed liquor is hereinafter, be added
80mL H2O2, until bubble-free generates in flask, reaction terminates.The color of reaction product gradually becomes glassy yellow from dark-brown, obtains
To mixed solution C.Mixed solution C is separated by centrifuge separation mode, centrifugation time 4min, revolving speed 7000r/min, into
Row a small amount of deionized water is added after being separated by solid-liquid separation and products therefrom is added in bag filter (bag filter pre-processes: by bag filter plus
Work is 20cm length cell, and heats 10min in the hot water, and cooling is spare), upper lower sealing is sealed, then put it into be full of and go
It dialyses in the sink of ionized water, is examined with pH analyzer, as pH=7, dialysis is completed, by the graphene oxide after dialysis
It is added after appropriate amount of deionized water is freeze-dried and prepares the graphene oxide dispersion of 1g/L；
Step 3: nickel foam substrate being put into the mixed liquor of step 2 formation and do anode, and graphite plate does cathode, connection electricity
Source carries out electrochemical deposition, and deposition voltage 3.0V, sedimentation time 30min obtain pure PPy/GO combination electrode.
As shown in Figure 1, according to Fig. 1 (a) and Fig. 1 (b) it is found that the surface topography of nickel foam is changed after introducing GO,
Surface forms apparent composite deposite, forms ball bumps and 3 D stereo duct structure.PPy is spherical in shape and uniformly divides
Cloth is in the GO lamella that porous and height is peeled off.In addition, GO piece is connected with each other, the specific surface area of electrode material is improved, is helped
In diffusion absorption of the ion in electrode material.Therefore, infer that the introducing of GO can significantly improve the absorption property of electrode.Pass through this
Capacitive deionization PPy/GO combination electrode made from the preparation method of invention can have the waste water containing heavy metal ion
Effect absorption.
PPy/GO composite material is as follows to the Electro Sorb process of heavy metal wastewater thereby:
Electrical conductivity of solution is measured using conductivity meter, electrode is the PPy/GO composite material of experiment preparation, simulates heavy metal
Waste water is copper, aluminium, zinc, the one or more mixed solution such as nickel and lead；
Firstly, to 200mL concentration be 100mgL-1Cu2+PPy/GO composite material is placed in solution, then carries out magnetic force
Stirring；
Then, clamping voltage 1.2V is set, electrical conductivity of solution is tested by conductivity meter, it is primary every 1min record, make
Electrolyte reaches absorption-desorption balance.
As shown in Fig. 2, being pure PPy electrode and PPy/GO combination electrode the Electro Sorb Cu obtained of the embodiment of the present invention 22+When
Adsorption saturation curve.As shown in Figure 2, after GO is added, the electro adsorption capacity of electrode is significantly improved；
As shown in figure 3, being the PPy/GO combination electrode Electro Sorb various concentration Cu obtained of the embodiment of the present invention 22+When inhale
Attached amount versus time curve.As seen from the figure, work as Cu2+Concentration is 80mgL-1When Electro Sorb efficiency highest.
As shown in figure 4, being the PPy/GO combination electrode Electro Sorb Cu obtained of the embodiment of the present invention 22+Shi Butong absorption electricity
Depress adsorbance versus time curve.As seen from the figure, the electro adsorption capacity of PPy/GO combination electrode with voltage increase
And it gradually increases, the Electro Sorb efficiency highest in 1.6V.
As shown in figure 5, the PPy/GO combination electrode obtained for the embodiment of the present invention 2 has carried out 5 adsorption/desorption circulations
Experiment.As seen from the figure, 5 times circulation after regeneration rate up to 98% or so.PPy/GO combination electrode superperformance can keep multiple
Circulate operation.
As shown in fig. 6, the X ray diffracting spectrum of the GO obtained for the embodiment of the present invention 2.As seen from the figure, at 11.02 °
For the characteristic peak of GO, crystal face is (001), consistent with document report.
Fig. 8 is the PPy/GO combination electrode obtained of the embodiment of the present invention 2 to Ag+,Cu2+,Pb2+,Cd2+And Fe3+Five kinds of gold
Belong to the saturated extent of adsorption of ion.As seen from the figure, PPy/GO combination electrode is to Fe3+Adsorption capacity highest, to Ag+Adsorption capacity
It is minimum, respectively 44.37mg/g and 30.26mg/g.Therefore, the PPy/GO combination electrode ionic adsorption amount high to valence state is bigger.
Combination electrode is to bivalent metal ion (Cu2+,Pb2+And Cd2+) adsorption capacity be respectively 41.51mg/g, 38.68mg/g and
36.59mg/g。
Embodiment described above is only that preferred embodiment of the invention is described, and is not carried out to the scope of the present invention
It limits, without departing from the spirit of the design of the present invention, those of ordinary skill in the art make technical solution of the present invention
Various changes and improvements, should all fall into claims of the present invention determine protection scope in.
Claims (10)
1. a kind of preparation method of PPy/GO combination electrode, it is characterised in that: the following steps are included:
Step 1: pyrrole monomer is added in neopelex solution and stirs evenly, obtains finely dispersed mixing
Liquid A；
Step 2: graphene oxide dispersion being added into step 1 mixed liquor A, and ultrasonic disperse to uniform state is dispersed
Uniform mixed solution B；
Step 3: using nickel foam as anode, homalographic graphite plate makees electricity as cathode, with mixed solution B described in step 2
Liquid is solved, electrochemical deposition is carried out and obtains PPy/GO complex capacitance deionization electrode material.
2. a kind of preparation method of PPy/GO combination electrode according to claim 1, it is characterised in that: 12 in step 1
The volume ratio of alkyl benzene sulphonate sodium solution and pyrrole monomer is 500:7, mixing time 20min.
3. a kind of preparation method of PPy/GO combination electrode according to claim 1, it is characterised in that: in step 2, oxygen
Graphite alkene dispersion liquid the preparation method is as follows:
3g NaNO is added in 500mL round-bottomed flask3, 3g graphite and the dense H of 100mL2SO4, persistently it is stirred to react in ice-water bath
30min, by 9g KMnO4Flask is added under stiring, then removes ice bath, mixed solution persistently stirs 1h at 35 DEG C, then
100mL double distilled water is added, 90 DEG C of the temperature holding of mixed liquor is hereinafter, be added 80mL H2O2, until bubble-free generates in flask, instead
It should terminate, the color of reaction product gradually becomes glassy yellow from dark-brown, obtains mixed solution C, and mixed solution C is centrifugated,
Centrifugation time 4min, revolving speed 7000r/min are added deionized water and products therefrom are added by pre- after being separated by solid-liquid separation
In the bag filter of processing, upper lower sealing is sealed, then puts it into the sink full of deionized water and dialyses, with pH analyzer
It examines, as pH=7, dialysis is completed, and the graphene oxide after dialysis is added after appropriate amount of deionized water is freeze-dried and is matched
The graphene oxide dispersion of 1g/L is made.
4. a kind of preparation method of PPy/GO combination electrode according to claim 1, it is characterised in that: aoxidized in step 2
The volume ratio of graphene dispersing solution and mixed liquor A is 1:1.
5. a kind of preparation method of PPy/GO combination electrode according to claim 1, it is characterised in that: ultrasonic in step 2
Power is 200W, ultrasonic time 10min.
6. a kind of preparation method of PPy/GO combination electrode according to claim 3, it is characterised in that: bag filter pretreatment
Process are as follows: bag filter is processed as 20cm length cell, and heats 10min in the hot water, cooling is spare.
7. a kind of preparation method of PPy/GO combination electrode according to claim 1, it is characterised in that: under room temperature,
Electrochemical deposition voltage is 3.0V, sedimentation time 25min, is stirred in deposition process to electrolyte.
8. a kind of PPy/GO combination electrode material that preparation method according to claim 1-7 is prepared.
9. a kind of application in absorption waste water of PPy/GO combination electrode material according to any one of claims 8.
10. a kind of application in absorption waste water of PPy/GO combination electrode material according to claim 9, feature exist
In: the waste water is the waste water containing heavy metal.
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| CN115465924B (en) * | 2022-09-19 | 2024-03-26 | 西安泰金新能科技股份有限公司 | PPy/GO/MnO 2 Nano composite electrode, preparation method and application |
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