CN109678142A - A kind of function dough porous graphene and preparation method thereof - Google Patents
A kind of function dough porous graphene and preparation method thereof Download PDFInfo
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- CN109678142A CN109678142A CN201811581769.1A CN201811581769A CN109678142A CN 109678142 A CN109678142 A CN 109678142A CN 201811581769 A CN201811581769 A CN 201811581769A CN 109678142 A CN109678142 A CN 109678142A
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- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
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- C01B32/19—Preparation by exfoliation
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- C—CHEMISTRY; METALLURGY
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- C01B32/00—Carbon; Compounds thereof
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Abstract
The invention belongs to grapheme material fields, and disclose a kind of function dough porous graphene and preparation method thereof.For this method using the mixed solution of phytic acid and ammonium sulfate as electrolyte, graphite foil constitutes two electrolysis systems as cathode as anode, platinized platinum；DC power supply is used to provide Dc bias for the anode, the graphite foil expansion removing of the anode forms graphene under bias, and is discharged into the electrolyte；Filtering removes impurity after carrying out ultrasound to electrolyte, is then centrifuged and is chosen supernatant liquor for obtained filtrate, obtains the suspension of function dough porous graphene, and suspension filtering is finally obtained the function dough porous graphene.The present invention selects phytic acid as electrolyte, advantageously forms the hole graphene with vacancy defect, and can also introduce Yang Lin functional group, forms function dough porous graphene；Ammonium sulfate can promote the removing of graphite foil simultaneously, and the less graphene of the number of plies is made.
Description
Technical field
The invention belongs to grapheme material fields, more particularly, to a kind of function dough porous graphene and its preparation
Method.
Background technique
Graphene is to carry out the two-dimentional carbon material that honeycomb arrangement is constituted by single layer of carbon atom, since it has higher conductance
Rate, excellent mechanical stability and biggish theoretical specific surface area are used as the ideal of energy storage device such as battery, supercapacitor
Electrode material.
But by taking the micro- supercapacitor of film as an example, the extensive use of simple graphene-based micro- supercapacitor is limited to it
Relatively low capacity and energy density.This is because graphene layer between there are stronger Van der Waals for, lead to graphite
Alkene piece, which is easy to stack, reunites, so that hindering electrolyte enters electrode interior space, reduces ion transmission efficiency and electrode is effective
Specific surface area finally makes the performance of graphene-based supercapacitor bad.
Hole configurations is introduced on graphene basal plane can effectively solve the problems, such as this, prepare the side of porous graphene at present
Method specifically includes that catalytic oxidation, by spreading a large amount of catalyst granules on graphene basal plane, then selective paraffin oxidation catalyst
Adhering zone obtains porous graphene, and this method needs many more manipulations, and is easy to generate larger crack on the surface of the material；In the least
Micro light carving method is etched by superlaser, forms micropore on the surface of graphene, and this method can produce array and be uniformly distributed
Hole configurations, but it is with high costs, be unfavorable for manufacturing on a large scale；Snead process in air, with certain in air atmosphere
Temperature heats graphene powder, and amorphous areas is preferential on graphene basal plane and oxygen reaction generates CO2Evolution forms hole knot
Structure, this method is simple and easy, but needs previously prepared graphene finished product, and inevitably by graphene large area oxygen
Change.
Summary of the invention
For the disadvantages mentioned above and/or Improvement requirement of the prior art, the present invention provides a kind of function dough porous graphites
Alkene and preparation method thereof, wherein the preparation method is by electrochemical stripping method, using phytic acid and ammonium sulfate mixed solution as being electrolysed
Liquid realizes the preparation of function dough porous graphene.
To achieve the above object, according to one aspect of the present invention, a kind of system of function dough porous graphene is proposed
Preparation Method, which is characterized in that this method comprises the following steps:
(a) using the mixed solution of phytic acid and ammonium sulfate as electrolyte, graphite foil is as anode, and platinized platinum is as cathode, structure
At two electrolysis systems；
(b) in two electrolysis systems of step (a), DC power supply is used to provide Dc bias for the anode,
The graphite foil expansion removing of the anode forms graphene under bias effect, and is discharged into the electrolyte；
(c) electrolyte containing graphene for obtaining step (b) carries out ultrasound, filters off removal of impurities after making graphene dispersion
Then obtained filtrate is centrifuged and is chosen supernatant liquor by matter, obtain the suspension of function dough porous graphene, finally
Suspension filtering is obtained into the function dough porous graphene.
As it is further preferred that the concentration of phytic acid is preferably 0.02mol/L~0.04mol/L in the electrolyte.
As it is further preferred that the concentration of ammonium sulfate is preferably 0.08mol/L~0.12mol/L in the electrolyte.
As it is further preferred that the Dc bias is preferably+8V~+12V.
As it is further preferred that the time of the ultrasound is preferably 20min~40min.
As it is further preferred that the revolving speed of the centrifugation is preferably 3000r/min~6000r/min.
As it is further preferred that the time of the centrifugation is preferably 15min~25min.
It is another aspect of this invention to provide that providing a kind of function dough porous graphene prepared using the above method.
In general, through the invention it is contemplated above technical scheme is compared with the prior art, mainly have below
Technological merit:
1. the present invention selects phytic acid as electrolyte, the oxidation of graphite foil anode may advantageously facilitate, so that removing obtained
There are a large amount of amorphous areas for graphene, these regions are further selectively oxidized under the bias effect of anode, and are generated
Carbon oxide gas evolution, to form the hole graphene with vacancy defect；And phytic acid is as a kind of rich in oxygen phosphorus member
The organic acid of element, increases the hydrogen ion concentration in electrolyte after hydrolysis, can speed up stripping process, while also to production
Yang Lin functional group is introduced in object, is capable of forming function dough porous graphene；The Yang Lin functional group can provide fake capacitance,
It is exactly the functional group as faraday's redox reaction, increases material specific capacity, secondly graphite ene product can be made in water
In it is evenly dispersed, be conducive to liquid phase processing；
2. simultaneously, ammonium sulfate is added in the present invention in the electrolytic solution, the removing of graphite foil can be promoted, it is less that the number of plies is made
Graphene reduces ion transmission efficiency reduction caused by it reunites because of graphene stacking and asks with what electrode effective ratio area reduced
Topic；
3. especially, phytic acid concentration it is excessively high to will cause oxygen content in product too low and reduce its electric conductivity, and phytic acid concentration
It is too low, it is not easy to form porous structure, therefore phytic acid concentration is preferably 0.02mol/L~0.04mol/L in electrolyte；Sulphur simultaneously
The excessively high oxidation that can inhibit graphite foil of sour ammonium concentration, concentration is too low it will cause graphite foil removing is insufficient, therefore electrolyte
Middle ammonium sulfate concentrations are preferably 0.08mol/L~0.12mol/L；In addition, the too low meeting of direct current power source voltage so that peeling rate compared with
Slowly it or cannot remove, overtension can then make peeling rate too fast and keep the product number of plies more, and be easy to cause excessively
Oxidation is so that higher its electric conductivity of influences of the oxygen content of product, therefore Dc bias preferably+8~+12V, in above-mentioned suitable item
Function dough porous graphene obtained has hole configurations abundant under part, and electric conductivity is higher；
4. preparing function dough porous graphene not only time-saving and efficiency, low in cost, energy using method provided by the invention
It is enough to realize large-scale production, and product obtained has the advantage that hole is more, the number of plies is few and loads Yang Lin functional group, especially
It is suitable as the electrode material of supercapacitor, the capacity of capacitor can be effectively improved.
Detailed description of the invention
Fig. 1 is the preparation facilities figure of function dough porous graphene provided by the invention；
Fig. 2 (a)~(b) is the transmission electron microscopy of function dough porous graphene C-1 prepared by the embodiment of the present invention 1
Figure；
Fig. 3 is that function dough porous graphene C-1 prepared by the embodiment of the present invention 1 passes through after water filling1H nuclear magnetic resonance
Wave spectrogram；
Fig. 4 is the x-ray photoelectron spectroscopy figure of function dough porous graphene C-1 prepared by the embodiment of the present invention 1；
Fig. 5 is the X-ray light of the high-resolution P elements of function dough porous graphene C-1 prepared by the embodiment of the present invention 1
Electronic energy spectrum；
Fig. 6 is the Raman spectrogram of function dough porous graphene C-1 prepared by the embodiment of the present invention 1.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, with reference to the accompanying drawings and embodiments, right
The present invention is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, and
It is not used in the restriction present invention.As long as in addition, technical characteristic involved in the various embodiments of the present invention described below
Not constituting a conflict with each other can be combined with each other.
As shown in Figure 1, the present invention provides a kind of preparation methods of function dough porous graphene, which is characterized in that should
Method includes the following steps:
(a) using the mixed solution of phytic acid and ammonium sulfate as electrolyte, having a size of 1cm × 2cm~1cm × 4cm graphite
Foil forms two electrolysis systems as cathode, assembling as anode, platinized platinum, and phytic acid concentration is preferably in the electrolyte
0.02mol/L~0.04mol/L, ammonium sulfate concentrations are 0.08mol/L~0.12mol/L；
(b) in two motor electrolysis systems of step (a), DC power supply is used to provide+8V~+12V direct current for anode
Bias, the graphite foil, which gradually expands to remove, under bias forms graphene, and is discharged into the electrolyte；
(c) ultrasound that the electrolyte containing graphene for obtaining step (b) carries out 20min~40min makes stone therein
Black alkene dispersion, then filtering removes impurity, and by obtained filtrate under conditions of revolving speed is 3000r/min~6000r/min
It is centrifuged 15min~25min, the suspension that supernatant liquor obtains function dough porous graphene is chosen, finally by the suspension mistake
Filter obtains the function dough porous graphene.
It is another aspect of this invention to provide that providing a kind of function dough porous graphene prepared using the above method.
Embodiment 1
(a) using the mixed solution that phytic acid concentration is 0.03mol/L, ammonium sulfate concentrations are 0.1mol/L as electrolyte, ruler
The very little graphite foil for 1cm × 3cm forms two electrolysis systems as cathode, assembling as anode, platinized platinum；
(b) DC power supply is used to provide the Dc bias of+10V for anode, graphite foil gradually expands stripping under bias
From formation graphene, and it is discharged into the electrolyte；
(c) ultrasound that the electrolyte containing graphene for obtaining step (b) carries out 30min makes graphite foil therein point
It dissipates, then with the repeated filtration cleaning of cellulose mixture film, removes residual impurity, and be 4500r/ in revolving speed by obtained filtrate
It is centrifuged 20min under conditions of min, the suspension that supernatant liquor obtains function dough porous graphene is chosen, finally by the suspension
Liquid filtering obtains the function dough porous graphene, is denoted as C-1.
Obtained function dough porous graphene C-1 is subjected to transmission electron microscope test, obtained result such as Fig. 2 (a)
Shown in~(b), it is several nanometers that the surface of the C-1, which has diameter, and the micropore that size is inhomogenous；Fig. 3 is the C-1 by note
After water1H NMR spectrum figure, wherein peak A indicates that water exists in the form of block, and peak B indicates that water is present in graphene layer
Between, and peak C indicates that water is present among the micropore of graphene basal plane, peak C reflects the big of hole relative to the chemical shift of peak A
Small, chemical shift is bigger, then aperture is smaller, this map illustrate gained C-1 on micropore diameter between 1~10nm, together
Transmission electron microscope result shown in Fig. 2 matches, it was demonstrated that the presence of micropore；
Fig. 4 is the x-ray photoelectron spectroscopy figure of the C-1, and as the result is shown in addition to the peak C1s, there are one the apparent peaks O1s
With a lesser peak P2p, shows in prepared graphene and introduce oxygen-containing functional group, phosphorous functional group；By to C-1
The x-ray photoelectron test for carrying out high-resolution P elements, as a result as shown in figure 5, P elements therein are in the form of P=O and P-O
It is present among graphene lattice；
Fig. 6 is the Raman spectrogram of the C-1, it is with tri- main peaks of D, G and 2D, the ratio at the peak D and the peak G as the result is shown
About 1.12, show among graphene lattice that there are a large amount of defect, such as vacancy defect, boundary defects etc., to verify
The presence of the C-1 Hole and functional group.
Embodiment 2
(a) using the mixed solution that phytic acid concentration is 0.02mol/L, ammonium sulfate concentrations are 0.12mol/L as electrolyte, ruler
The very little graphite foil for 1cm × 2cm forms two electrolysis systems as cathode, assembling as anode, platinized platinum；
(b) DC power supply is used to provide the Dc bias of+8V for anode, graphite foil gradually expands removing under bias
Graphene is formed, and is discharged into the electrolyte；
(c) ultrasound that the electrolyte containing graphene for obtaining step (b) carries out 20min makes graphite foil therein point
It dissipates, then with the repeated filtration cleaning of cellulose mixture film, removes residual impurity, and be 6000r/ in revolving speed by obtained filtrate
It is centrifuged 15min under conditions of min, the suspension that supernatant liquor obtains function dough porous graphene is chosen, finally by the suspension
Liquid filtering obtains the function dough porous graphene, is denoted as C-2.
Through transmission electron microscope test and x-ray photoelectron spectroscopy test find the C-2 have it is nanometer level microporous and
Yang Lin phosphorus functional group.
Embodiment 3
(a) using the mixed solution that phytic acid concentration is 0.04mol/L, ammonium sulfate concentrations are 0.08mol/L as electrolyte, ruler
The very little graphite foil for 1cm × 4cm forms two electrolysis systems as cathode, assembling as anode, platinized platinum；
(b) DC power supply is used to provide the Dc bias of+12V for anode, graphite foil gradually expands stripping under bias
From formation graphene, and it is discharged into the electrolyte；
(c) ultrasound that the electrolyte containing graphene for obtaining step (b) carries out 40min makes graphite foil therein point
It dissipates, then with the repeated filtration cleaning of cellulose mixture film, removes residual impurity, and be 3000r/ in revolving speed by obtained filtrate
It is centrifuged 25min under conditions of min, the suspension that supernatant liquor obtains function dough porous graphene is chosen, finally by the suspension
Liquid filtering obtains the function dough porous graphene, is denoted as C-3.
Through transmission electron microscope test and x-ray photoelectron spectroscopy test find the C-3 have it is nanometer level microporous and
Yang Lin functional group.
As it will be easily appreciated by one skilled in the art that the foregoing is merely illustrative of the preferred embodiments of the present invention, not to
The limitation present invention, any modifications, equivalent substitutions and improvements made within the spirit and principles of the present invention should all include
Within protection scope of the present invention.
Claims (8)
1. a kind of preparation method of function dough porous graphene, which is characterized in that this method comprises the following steps:
(a) using the mixed solution of phytic acid and ammonium sulfate as electrolyte, graphite foil constitutes two as cathode as anode, platinized platinum
Electrolysis system；
(b) in two electrolysis systems of step (a), DC power supply is used to provide Dc bias for the anode, in bias
The graphite foil expansion removing of the anode forms graphene under effect, and is discharged into the electrolyte；
(c) electrolyte containing graphene for obtaining step (b) carries out ultrasound, makes filtering removal impurity after graphene dispersion,
Then obtained filtrate is centrifuged and is chosen supernatant liquor, obtain the suspension of function dough porous graphene, finally will
Suspension filtering obtains the function dough porous graphene.
2. the preparation method of function dough porous graphene as described in claim 1, which is characterized in that planted in the electrolyte
The concentration of acid is preferably 0.02mol/L~0.04mol/L.
3. the preparation method of function dough porous graphene as claimed in claim 1 or 2, which is characterized in that the electrolyte
The concentration of middle ammonium sulfate is preferably 0.08mol/L~0.12mol/L.
4. the preparation method of function dough porous graphene as claimed in any one of claims 1 to 3, which is characterized in that described
Dc bias is preferably+8V~+12V.
5. such as the preparation method of the described in any item function dough porous graphenes of Claims 1 to 4, which is characterized in that described
The time of ultrasound is preferably 20min~40min.
6. the preparation method of function dough porous graphene as claimed in any one of claims 1 to 5, which is characterized in that described
The revolving speed of centrifugation is preferably 3000r/min~6000r/min.
7. the preparation method of function dough porous graphene as described in any one of claims 1 to 6, which is characterized in that described
The time of centrifugation is preferably 15min~25min.
8. a kind of function dough porous graphene using such as the method preparation of any one of claim 1~7.
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| CN115676819A (en) * | 2021-07-21 | 2023-02-03 | 比亚迪股份有限公司 | Graphite material preparation method, graphite material and power battery |
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