CN110316729A - A method of graphene is prepared based on high concentration aqueous solutions of organic salts electrochemical intercalation - Google Patents
A method of graphene is prepared based on high concentration aqueous solutions of organic salts electrochemical intercalation Download PDFInfo
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- CN110316729A CN110316729A CN201910747764.XA CN201910747764A CN110316729A CN 110316729 A CN110316729 A CN 110316729A CN 201910747764 A CN201910747764 A CN 201910747764A CN 110316729 A CN110316729 A CN 110316729A
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- C01B32/19—Preparation by exfoliation
Abstract
The present invention provides a kind of methods for preparing graphene based on high concentration aqueous solutions of organic salts electrochemical intercalation, belong to technical field of graphene preparation.The present invention is using high concentration aqueous solutions of organic salts as electrolyte, using graphite as anode, using inertia conductive noble metal material as cathode, carries out electrochemical intercalation reaction, obtains graphenes aggregations.The present invention uses high concentration aqueous solutions of organic salts as electrolyte, is able to suppress the fast decoupled of water, and graphite may be implemented continues controllable intercalation.Simultaneously, organic salt in the present invention is fluorine-containing macromolecular organic salt, still there is stable structure under voltage effect, the chemical reaction of intercalating ions and graphite can be effectively avoided in electrochemical intercalation reaction process, the crystalline structure of graphite is kept not to be damaged, so that the graphene of high quality be prepared.Preparation method short preparation period provided by the invention, it is at low cost, acid solution is not generated, environmental-friendly, method is simple, it is easy to accomplish industrial mass production.
Description
Technical field
The present invention relates to technical field of graphene preparation, in particular to a kind of to be based on high concentration aqueous solutions of organic salts electrochemistry
The method that intercalation prepares graphene.
Background technique
From the study group of the leader of University of Manchester A.K.Geim in 2004 propose the concept of graphene (Graphene) with
Come, an other bright star of the graphene as carbon family has obtained the great attention of physics, chemistry and material scholar.
Up to the present, domestic and international scientific research personnel conducts extensive research the preparation of graphene, wherein electrification
Removing intercalation prepares the technology of graphene because its cheap cost and shirtsleeve operation are by more extensive concern.However
Traditional electrochemistry is to realize intercalation and removing on the electrode using the bubble of ion and generation in electrolyte, because
This causes the serious destruction of graphite electrode with the carry out electrolyte decomposition aggravation of intercalation and removing, once carbon paper is in electricity
Extremely upper to peel off into solution, intercalation stripping process stops, if without realizing that intercalation will well before peeling
The uncontrollable problem of the graphene number of plies being prepared is caused, and since oxidation reaction occurring between intercalating ions and graphite,
The crystal structure of graphene can further be influenced.Therefore, how effectively to control the reaction of intercalation extruding ensures continuing for graphite
Intercalation and controllable extruding, and control the oxidation reaction of intercalating ions and graphite, be current critical issue urgently to be solved.
Summary of the invention
Stone is prepared based on high concentration aqueous solutions of organic salts electrochemical intercalation in view of this, it is an object of that present invention to provide one kind
The method of black alkene.Preparation method provided by the invention is able to achieve the lasting intercalation to graphite, and gained graphene number of plies is controllable, crystal
Structure is not destroyed.
In order to achieve the above-mentioned object of the invention, the present invention the following technical schemes are provided:
The present invention provides a kind of methods for preparing graphene based on high concentration aqueous solutions of organic salts electrochemical intercalation, including
Following steps:
Using high concentration aqueous solutions of organic salts as electrolyte, using graphite as anode, with inertia conductive noble metal material work
For cathode, electrochemical intercalation reaction is carried out, graphenes aggregations are obtained；
Mass concentration >=50% of organic salt in the high concentration aqueous solutions of organic salts；Or the high concentration organic salt is water-soluble
Volumetric concentration >=50% of organic salt in liquid；
The organic salt is double trifluoromethanesulfonimide salt and/or fluoroform sulphonate.
Preferably, the graphite is one or more of natural flake graphite, oriented graphite, graphite paper and graphite rod.
Preferably, the material of the inertia conductive noble metal material is platinum or silver.
Preferably, double trifluoromethanesulfonimide salt are double trifluoromethanesulfonimide lithiums, double fluoroform sulphonyl
One or more of imines sodium and double trifluoromethanesulfonimide zinc, the fluoroform sulphonate are trifluoromethanesulfonic acid lithium, three
One or more of fluorine methanesulfonic sodium and trifluoromethanesulfonic acid zinc.
Preferably, the spacing between the anode and cathode is 1~10cm.
Preferably, the voltage that the electrochemical intercalation reaction applies is 5~30V.
Preferably, the time of the electrochemical intercalation reaction is 0.5~3h, the temperature of electrolyte when electrochemical intercalation is reacted
It is 10~35 DEG C.
It preferably, further include that graphenes aggregations are post-processed after the electrochemical intercalation reaction, the post-processing
The following steps are included:
It is successively washed after the graphenes aggregations are separated, is ultrasonic and dry, obtaining graphene powder.
Preferably, the power of the ultrasound is 80~150W, and the time is 0.5~2h.
Preferably, the temperature of the drying is -40~-20 DEG C, and the time is 24~72h.
The present invention provides a kind of method for preparing graphene based on high concentration aqueous solutions of organic salts electrochemical intercalation, this hairs
It is bright using high concentration aqueous solutions of organic salts as electrolyte, using graphite as anode, using inertia conductive noble metal material as cathode,
Electrochemical intercalation reaction is carried out, to obtain graphenes aggregations.The present invention uses high concentration aqueous solutions of organic salts as electrolysis
Liquid is able to suppress the fast decoupled of water using the hydrated salt structure of water content less in electrolyte and high concentration organic salt,
Graphite may be implemented continues controllable intercalation.Meanwhile the organic salt in the present invention is fluorine-containing macromolecular organic salt, is made in voltage
Still there is stable structure under, the chemistry of intercalating ions and graphite can be effectively avoided in electrochemical intercalation reaction process
Reaction, keeps the crystalline structure of graphite not to be damaged, so that the graphene of high quality be prepared.Preparation side provided by the invention
Method short preparation period, it is at low cost, acid solution is not generated, environmental-friendly, method is simple, it is easy to accomplish industrial mass production.
Detailed description of the invention
Fig. 1 is the pictorial diagram of 1 gained graphenes aggregations of embodiment；
Fig. 2 is the stereoscan photograph of 1 gained graphene powder of embodiment；
Fig. 3 is the X ray diffracting spectrum of 2 gained graphene powder of embodiment；
Fig. 4 is the stereoscan photograph of 1 gained graphite clast of comparative example；
Fig. 5 is the pictorial diagram of the resulting graphite clast of comparative example 2.
Specific embodiment
The present invention provides a kind of methods for preparing graphene based on high concentration aqueous solutions of organic salts electrochemical intercalation, including
Following steps:
Using high concentration aqueous solutions of organic salts as electrolyte, using graphite as anode, with inertia conductive noble metal material work
For cathode, electrochemical intercalation reaction is carried out, graphenes aggregations are obtained.
In the present invention, in the high concentration aqueous solutions of organic salts organic salt mass concentration >=50%, preferably >=60%；
Or in the high concentration aqueous solutions of organic salts organic salt volumetric concentration >=50%, preferably >=60%；In the present invention, described double
Trifluoromethanesulfonimide salt is double trifluoromethanesulfonimide lithiums, double trifluoromethanesulfonimide sodium and double fluoroform sulphonyl
One or more of imines zinc, the fluoroform sulphonate are trifluoromethanesulfonic acid lithium, trifluoromethanesulfonic acid sodium and trifluoromethanesulfonic acid
One or more of zinc.
In the present invention, the volume of the electrolyte and the mass ratio of graphite are preferably 10~40:1, more preferably 20~
30:1.By the present invention in that using high concentration aqueous solutions of organic salts as electrolyte, wherein high concentration aqueous solutions of organic salts being capable of shape
At a kind of hydration salt system, the present invention utilizes the hydrated salt structure of water content and high concentration organic salt less in electrolyte,
It is able to suppress the fast decoupled of water, graphite may be implemented continues controllable intercalation.Meanwhile the organic salt in the present invention has stabilization
Structure, the chemical reaction of intercalating ions and graphite can be effectively avoided in electrochemical intercalation reaction process, keeps graphite
Crystalline structure is not damaged, so that the graphene of high quality be prepared.
In the present invention, the graphite is preferably one of natural flake graphite, oriented graphite, graphite paper and graphite rod
Or it is several；The material of the inertia conductive noble metal material is preferably platinum or silver, is particularly preferred as in platinized platinum, platinum filament and filamentary silver
It is one or more of.The present invention does not have special requirement to the source of the graphite and conductive noble metal material, normal using this field
Advise commercially available above-mentioned material.
In the present invention, the electrochemical intercalation reaction preferably carries out in the system of opening wide；Between the anode and cathode
Spacing is preferably 1~10cm, more preferably 4~8cm.The present invention is adjustable to have by the spacing between control anode and cathode
For machine saline solution to the intercalation rate of graphite, the two spacing is smaller, and intercalation rate is faster.In the present invention, the electrochemistry is inserted
The voltage that layer reaction applies is preferably 5~30V, more preferably 10~20V；The voltage of the application is preferably DC voltage, this
The voltage that invention is applied by control, can peel off too early to avoid graphite, guarantee duration and the speed of graphite intercalation.At this
In invention, the time of the electrochemical intercalation reaction is preferably 0.5~3h, more preferably 1~2h, the electrochemical intercalation reaction
When electrolyte temperature be preferably 10~35 DEG C, more preferably 20~30 DEG C.In the present invention, gained graphenes aggregations are specific
For the aggregation of two-dimensional slice graphene, which has complete orderly structure and big particle size, the graphene
The size of aggregation preferably >=300 μm.
The present invention further preferably includes post-processing to graphenes aggregations after electrochemical intercalation reaction, described
Post-processing the following steps are included:
It is successively washed after the graphenes aggregations are separated, is ultrasonic and dry, obtaining graphene powder.
In the present invention, the isolated mode preferably filters, and the washing is preferably high purity water with detergent.This hair
The bright pH=7 for making graphenes aggregations by washing.Graphenes aggregations after washing are preferably placed in high purity water by the present invention
The mass ratio of progress ultrasound, the graphenes aggregations and high purity water is preferably 5~10:1, more preferably 6~8:1；In this hair
In bright, the power of the ultrasound is preferably 80~150W, and more preferably 100~120W, the time is preferably 0.5~2h, more preferably
For 1~1.5h；The ultrasound is preferably supersonic cleaning machine with equipment.In the present invention, graphenes aggregations are become by ultrasound
The graphene dispersing solution of two-dimensional slice.In the present invention, the drying is preferably freeze-dried, and the temperature of the drying is preferred
It is -40~-20 DEG C, more preferably -35~-25 DEG C, the time is preferably 24~72h, more preferably 36~60h, and the freezing is dry
Dry vacuum degree is preferably 20Pa.
Preparation method short preparation period provided by the invention, it is at low cost, acid solution is not generated, environmental-friendly, method is simple, easily
In realization industrial mass production.
Graphite is prepared based on high concentration aqueous solutions of organic salts electrochemical intercalation to provided by the invention below with reference to embodiment
The method of alkene is described in detail, but they cannot be interpreted as limiting the scope of the present invention.
Embodiment 1
Using double trifluoromethanesulfonimide lithiums as electrolyte, weighs the bis- trifluoromethanesulfonimide lithiums of 18.09g and 3g is added
Water (mass concentration of organic salt be 85.8%) solution 30min is placed in 50 DEG C of baking ovens, it is as clear as crystal as electricity to solution
It solves liquid and is used for electrochemical intercalation graphite.Prepared electrolyte is added in a cell, choosing graphite paper is anode and direct current
Source is connected, and is connected using platinized platinum as cathode with DC power supply, and two electrodes apply the voltage of 20V at a distance of 5cm, at 25 DEG C
Intercalation expands sustainable 3h electrode and does not peel off, obtains graphenes aggregations, pictorial diagram is as shown in Figure 1, by vacuum mistake
After filtering is washed, disperses 30min in the supersonic cleaning machine of 80W and obtain graphene dispersing solution, dispersion liquid vacuum under the conditions of -20 DEG C
Degree 20Pa is dry, and graphene powder is prepared in 72h.
Electronic Speculum (SEM) analysis is scanned to gained graphene powder, gained stereoscan photograph is as shown in Figure 2.By Fig. 2
It is found that present invention gained Graphene powder tailpiece diameter size>50 μm, thickness<5nm.
Embodiment 2
Using double trifluoromethanesulfonimide lithiums as electrolyte, weighs the bis- trifluoromethanesulfonimide lithiums of 5mL and be added 1mL's
Water (volumetric concentration of organic salt is 83.3%), places solution 30min in 50 DEG C of baking ovens, as clear as crystal as highly concentrated to solution
Saline electrolysis liquid is used for electrochemical intercalation graphite.Be added prepared electrolyte in a cell, choose graphite paper be anode with
DC power supply is connected, and is connected using platinum filament as cathode with DC power supply, and two electrodes apply the voltage of 15V at a distance of 8cm,
Intercalation expands sustainable 1h electrode and does not peel off at 10 DEG C, obtains graphenes aggregations, after vacuum filter is cleaned,
Disperse 1h in the supersonic cleaning machine of 100W and obtain graphene dispersing solution, dispersion liquid vacuum degree 20Pa under the conditions of -30 DEG C dries 72h
Graphene powder is prepared.
X-ray diffraction analysis is carried out to gained graphene powder, gained X ray diffracting spectrum is as shown in Figure 3.It can by Fig. 3
Know, present invention gained graphene powder typical graphene diffraction maximum occurs at 25 degree or so.
Embodiment 3
With trifluoromethanesulfonic acid sodium (NaCF3SO3) it is used as electrolyte, weigh 4gNaCF3SO3Water (the matter of organic salt of 1g is added
Measure concentration be 80%) in 50 DEG C of baking ovens place solution 30min, to solution it is as clear as crystal as highly concentrated saline electrolysis liquid for electricity
Chemical graft graphite.Prepared electrolyte is added in a cell, choosing graphite paper is that anode is connected with DC power supply, with
Filamentary silver is connected as cathode with DC power supply, and two electrodes apply the voltage of 5V at a distance of 1cm, and intercalation expansion can be held at 35 DEG C
Continuous 2h electrode does not peel off, obtains graphenes aggregations, after vacuum filter is cleaned, divides in the supersonic cleaning machine of 120W
Scattered 30min obtains graphene dispersing solution, and Graphene powder is prepared in dispersion liquid vacuum degree 20Pa drying under the conditions of -40 DEG C for 24 hours
End.
Electron microscope analysis and X-ray diffraction analysis, acquired results and embodiment 1 and implementation are scanned to this graphene powder
Example 2 is similar.
Comparative example 1
Using double trifluoromethanesulfonimide lithiums (LITFSI) as electrolyte, weighing the water that 5g is added in 0.5gLITFSI (has
The mass concentration of machine salt is that solution 30min 9.09%) is placed in 50 DEG C of baking ovens, is used for the as clear as crystal conduct electrolyte of solution
Electrochemical intercalation graphite.Prepared electrolyte is added in a cell, choosing graphite paper is that anode is connected with DC power supply,
It is connected using platinum filament as cathode with DC power supply, two electrodes apply the voltage of 5V at a distance of 5cm, and intercalation carries out at 25 DEG C
Then occur apparent electrode when 5min and peel off and damage phenomenon, this is because the electrolyte of low concentration largely depositing due to water-soluble matter
Causing water electrolysis reaction for key reaction, the bubble generation of aggravation further damages the integrality of graphite anode, peels off
Graphite clast scanning electron microscope such as Fig. 4, it can be seen that since the peeling effect of premature exfoliated graphite is poor, graphite
Alkene lamella is very thick, thickness > 10nm, and comparison diagram 2 can not embody the translucent feature of graphene platelet.
Comparative example 2
Using sodium tetrafluoroborate as electrolyte, the water (mass concentration of organic salt is 66.7%) for weighing 10g addition 5g exists
Solution 30min is placed in 50 DEG C of baking ovens, is used for electrochemical intercalation graphite to the as clear as crystal conduct electrolyte of solution.In a cell
Prepared electrolyte is added, choosing graphite paper is that anode is connected with DC power supply, using platinum filament as cathode and DC power supply
It is connected, two electrodes apply the voltage of 5V at a distance of 5cm, and intercalation carries out then occurring apparent electrode peeling when 5min at 25 DEG C
With damage phenomenon, this is because the unstable easy decomposition under voltage effect of the anion of small molecule inorganic salts, the bubble of aggravation produce
Life further damages the integrality of graphite anode, and graphite then has begun off into solution knot during electricity peels off
The reaction of beam electric removing and intercalation, pictorial diagram with Fig. 1 as shown in figure 5, compare as can be seen that occurring in this solution
Excessive graphite clast.
Embodiment 4
With double trifluoromethanesulfonimide zinc Al (TFSI)3As electrolyte, the bis- trifluoromethanesulfonimide zinc of 3mL are weighed
The water (mass concentration of organic salt is 50%) of 3mL is added, solution 30min is placed in 50 DEG C of baking ovens, it is as clear as crystal to solution
Electrochemical intercalation graphite is used for as electrolyte.Be added prepared electrolyte in a cell, choose graphite paper be anode with
DC power supply is connected, and is connected using platinized platinum as cathode with DC power supply, and two electrodes apply the voltage of 10V at a distance of 10cm,
Intercalation expands sustainable 30min electrode and does not peel off at 25 DEG C, obtains graphenes aggregations, after vacuum filter is cleaned,
Disperse 1h in the supersonic cleaning machine of 150W and obtain graphene dispersing solution, dispersion liquid vacuum degree 20Pa under the conditions of -20 DEG C is dry
Graphene powder is prepared in 36h.
Electron microscope analysis and X-ray diffraction analysis, acquired results and embodiment 1 and implementation are scanned to this graphene powder
Example 2 is similar.
Embodiment 5
With trifluoromethanesulfonic acid zinc Zn (CF3SO3)3As electrolyte, 6mLZn (CF is weighed3SO3)3The water that 4mL is added is (organic
The volumetric concentration of salt be 60%) in 50 DEG C of baking ovens place solution 30min, to solution it is as clear as crystal as electrolyte for electrification
Learn intercalated graphite.Prepared electrolyte is added in a cell, choosing graphite paper is that anode is connected with DC power supply, with platinum
Piece is connected as cathode with DC power supply, and two electrodes apply the voltage of 8V at a distance of 3cm, and intercalation expansion is sustainable at 25 DEG C
80min electrode does not peel off, obtains graphenes aggregations, after vacuum filter is cleaned, divides in the supersonic cleaning machine of 80W
Scattered 30min obtains graphene dispersing solution, and dispersion liquid vacuum degree 20Pa under the conditions of -30 DEG C is dry, and Graphene powder is prepared in 72h
End.
Electron microscope analysis and X-ray diffraction analysis, acquired results and embodiment 1 and implementation are scanned to this graphene powder
Example 2 is similar.
As seen from the above embodiment, preparation method provided by the invention can be realized the lasting intercalation to graphite, gained stone
The black alkene number of plies is controllable, and crystal structure is not destroyed.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications are also answered
It is considered as protection scope of the present invention.
Claims (10)
1. a kind of method for preparing graphene based on high concentration aqueous solutions of organic salts electrochemical intercalation, which is characterized in that including with
Lower step:
Using high concentration aqueous solutions of organic salts as electrolyte, using graphite as anode, using inertia conductive noble metal material as yin
Pole carries out electrochemical intercalation reaction, obtains graphenes aggregations；
Mass concentration >=50% of organic salt in the high concentration aqueous solutions of organic salts；Or in the high concentration aqueous solutions of organic salts
Volumetric concentration >=50% of organic salt；
The organic salt is double trifluoromethanesulfonimide salt and/or fluoroform sulphonate.
2. the method according to claim 1, wherein the graphite is natural flake graphite, oriented graphite, graphite
One or more of paper and graphite rod.
3. the method according to claim 1, wherein the material of the inertia conductive noble metal material be platinum or
Silver.
4. the method according to claim 1, wherein double trifluoromethanesulfonimide salt are double fluoroforms
One or more of sulfimide lithium, double trifluoromethanesulfonimide sodium and double trifluoromethanesulfonimide zinc, the trifluoro
Mesylate is one or more of trifluoromethanesulfonic acid lithium, trifluoromethanesulfonic acid sodium and trifluoromethanesulfonic acid zinc.
5. the method according to claim 1, wherein the spacing between the anode and cathode is 1~10cm.
6. the method according to claim 1, wherein the electrochemical intercalation reaction apply voltage be 5~
30V。
7. the method according to claim 1, wherein the time of electrochemical intercalation reaction is 0.5~3h, electricity
The temperature of electrolyte is 10~35 DEG C when chemical graft reacts.
8. the method according to claim 1, wherein further including to graphene after electrochemical intercalation reaction
Aggregation is post-processed, it is described post-processing the following steps are included:
It is successively washed after the graphenes aggregations are separated, is ultrasonic and dry, obtaining graphene powder.
9. according to the method described in claim 8, it is characterized in that, the power of the ultrasound be 80~150W, the time be 0.5~
2h。
10. according to the method described in claim 8, it is characterized in that, the temperature of the drying be -40~-20 DEG C, the time 24
~72h.
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| CN110817961A (en) * | 2019-10-21 | 2020-02-21 | 厦门虹鹭钨钼工业有限公司 | Preparation method of molybdenum disulfide nanosheet material |
| CN111463524A (en) * | 2020-03-16 | 2020-07-28 | 中南大学 | Alkaline water-based electrolyte for aluminum-air battery and application thereof |
| CN113666367A (en) * | 2021-08-30 | 2021-11-19 | 山东恒华新材料有限公司 | Electrolytic tank for preparing graphite intercalation and preparation method of graphite intercalation |
| CN114408909A (en) * | 2022-03-02 | 2022-04-29 | 广西师范大学 | Method for preparing graphene by electrochemically stripping graphite |
| CN114433852A (en) * | 2022-03-14 | 2022-05-06 | 清华大学 | Method for preparing stibene nanosheet through electrochemical stripping |
| CN114956178A (en) * | 2022-04-08 | 2022-08-30 | 湖南大学 | Electrochemical stripping method of two-dimensional layered material |
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| CN108698050A (en) * | 2016-02-17 | 2018-10-23 | 纳米技术仪器公司 | Produce the electrochemical method of single layer or few layer graphene piece |
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| CN105152164A (en) * | 2015-08-21 | 2015-12-16 | 合肥工业大学 | Preparation method of graphene sheet |
| CN108698050A (en) * | 2016-02-17 | 2018-10-23 | 纳米技术仪器公司 | Produce the electrochemical method of single layer or few layer graphene piece |
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| CN110817961A (en) * | 2019-10-21 | 2020-02-21 | 厦门虹鹭钨钼工业有限公司 | Preparation method of molybdenum disulfide nanosheet material |
| CN110817961B (en) * | 2019-10-21 | 2022-06-14 | 厦门虹鹭钨钼工业有限公司 | Preparation method of molybdenum disulfide nanosheet material |
| CN111463524A (en) * | 2020-03-16 | 2020-07-28 | 中南大学 | Alkaline water-based electrolyte for aluminum-air battery and application thereof |
| CN111463524B (en) * | 2020-03-16 | 2021-11-05 | 中南大学 | Alkaline water-based electrolyte for aluminum-air battery and application thereof |
| CN113666367A (en) * | 2021-08-30 | 2021-11-19 | 山东恒华新材料有限公司 | Electrolytic tank for preparing graphite intercalation and preparation method of graphite intercalation |
| CN114408909A (en) * | 2022-03-02 | 2022-04-29 | 广西师范大学 | Method for preparing graphene by electrochemically stripping graphite |
| CN114408909B (en) * | 2022-03-02 | 2024-03-15 | 广西师范大学 | Method for preparing graphene by electrochemical stripping of graphite |
| CN114433852A (en) * | 2022-03-14 | 2022-05-06 | 清华大学 | Method for preparing stibene nanosheet through electrochemical stripping |
| CN114956178A (en) * | 2022-04-08 | 2022-08-30 | 湖南大学 | Electrochemical stripping method of two-dimensional layered material |
| CN114956178B (en) * | 2022-04-08 | 2023-08-08 | 湖南大学 | Electrochemical stripping method for two-dimensional layered material |
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