CN109594097A - The method of graphene quantum dot is prepared under electric field and ultrasonic field coupling - Google Patents
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Abstract
The invention discloses a kind of methods that graphene quantum dot is prepared under electric field and ultrasonic field coupling.The present invention has selected high pure graphite electrode cheap and easy to get for raw material, using disubstituted imidazole class ionic liquid as electrolyte, at room temperature, under the coupling of electric field and ultrasonic field, has prepared water-soluble graphene quantum dot.Graphite electrode of the present invention in the electrolyte, prepares graphene quantum dot under electric field and ultrasonic field coupling, and electrolyte is disubstituted imidazole class ionic liquid, and the method for the present invention green, environmental protection are simple, safe, have large-scale production potentiality.
Description
Technical field
The present invention relates to a kind of preparation methods of grapheme material, more particularly to a kind of preparation side of graphene quantum dot
Method is applied to carbon nanomaterial technical field.
Background technique
Graphene (Graphene) refers to planar monolayer carbon atom with sp2 hydridization, the bi-dimensional cellular shape for composition of combining closely
Hexagonal lattice material, this special structure impart the excellent performance of graphene.Since the connection between carbon atom is very soft
Tough, when there are external mechanical force, graphene planes meeting automatic bending deformation will not make carbon atom rearrangement.Therefore, graphite
Alkene can maintain the stabilization of structure always, become most hard material, and it is more than 100 times of steel that intensity, which reaches 130Gpa,.Graphene is flat
There are π track, the electronics of each carbon atom is in delocalization state, can move freely, therefore graphene has carbon atom in face
Superior thermal conductive property, thermal conductivity is up to 5000Wm-1·K-1；And in graphene planes electronics movement rate it is much high
Electronic movement velocity in general conductor is the most fast carbon material of current electronics conduction of velocity, and electric conductivity is excellent, carrier
Mobility reaches 15000cm2·V-1·S-1.In addition to this, graphene also has room-temperature quantum Hall effect, tunnel-effect and room temperature
The special natures such as ferromagnetism have just been concerned since emerging.
The size of grapheme material is micron order mostly, and quantization feature can be presented after its size reaches nanoscale, at
For graphene quantum dot.Only several or tens nano-scales single layer or few layer graphene quantum dot have extremely strong quantum
Effect shows many unique advantages, and if glow peak is regulated and controled by size, luminous efficiency is greatly enhanced.Moreover, graphene quantum dot
Nontoxicity, good biocompatibility can be equipped with functional group at its edge, answer in terms of biomarker, luminescent device, solar battery
With having a extensive future.The preparation method of graphene quantum dot is divided into two major classes at present: from top to bottom and bottom-to-top method.Patent
Application No. is the preparation methods of 201310222546.7 Chinese patent multicolor fluorescence graphene quantum dot material to disclose one kind
Pyrene grain surface is subjected to oxygen functionalization at low temperature, the water of low temperature is then carried out under the action of catalyst hydrazine hydrate and ammonium hydroxide
Surface-functionalized, the method that graphene quantum dot is prepared of hot dehydrogenation, growth and original position.The quantum dot of synthesis can be stablized point
Dissipate Yu Shuizhong, luminescent color or Wavelength tunable.But the invention is needed using nitric acid or dense sulfuric acid treatment, and oxidization time needs 20~
40 hours, after also need to carry out 24 hours hydrothermal reductions by the hydrazine hydrate of severe toxicity, severe reaction conditions, process is unrestrained
It is long.The preparation method for the Chinese patent high-efficient graphite alkene quantum dot that number of patent application is 201810370847.7 discloses a kind of logical
It crosses modified Hummer method and prepares graphite oxide, be then dispersed in water oxidation graphite solid, using high-speed shearing machine and surpass
Sound wave decentralized processing instrument handles graphite oxide suspension, finally adjusts graphite oxide solution pH to 10~11, is transferred to poly- four
In vinyl fluoride beaker, it is put into 120~250 DEG C of baking oven and toasts 0.5~2 hour.The method can quickly finish graphene quantum dot
Preparation, but there is still a need for largely use strong acid, highly basic and strong oxidizer.
Summary of the invention
In order to solve prior art problem, it is an object of the present invention to overcome the deficiencies of the prior art, and to provide one kind
The method that graphene quantum dot is prepared under electric field and ultrasonic field coupling, be able to achieve green, environmental protection, it is simple, safely prepare
Graphene quantum dot, raw material is cheap and easy to get, and preparation process is high-efficient, and the reaction time is short, and is able to achieve prepare with scale, has aobvious
The industrial value of work.
In order to achieve the above objectives, the present invention adopts the following technical scheme:
A method of graphene quantum dot being prepared under electric field and ultrasonic field coupling, is included the following steps:
A. disubstituted imidazole class ionic liquid is mixed with deionized water, compound concentration is the electrolysis of 0.1~0.3mol/L
Liquid；The disubstituted imidazole class ionic liquid preferably uses -3 methyl imidazolium tetrafluoroborate of 1- ethyl；
B. the electrolyte prepared in the step a is placed in electrolytic cell, with two graphite electrodes, is inserted in parallel into electrolysis
In liquid, electrochemical reaction appts are assembled, and using graphite electrode as carbon source raw material；It is preferred that keeping the distance of two graphite electrodes not low
In 3cm；
C. the electrolytic cell in the step b is put into ultrasonic pond, response voltage is arranged according to the type of ionic liquid,
Voltage value controls in the electrochemical window of the used ionic liquid of step a, and setting frequency is 0.05~1Hz, ultrasonic function
Rate is 30~90W, while applying electric field and ultrasonic field to electrolyte, under electric field and ultrasonic field coupling, carry out reaction 5~
10h obtains graphene quantum dot solution；It under electric field and ultrasonic field coupling, is preferably reacted, is made at room temperature
Standby graphene quantum dot solution；
D. by the step c acquired solution be filtered not higher than 0.22 μm of microporous barrier by aperture, by filtrate
3~5min of centrifugation is carried out with the speed of 10000~15000r/min, outwells supernatant, then will be added in the solid content of collection
Deionized water is washed, and is repeated as many times, until the pH value of solution after cleaning is neutrality, obtains the dispersion of graphene quantum dot
Liquid；
E. the dispersion liquid of the gained graphene quantum dot in the step d is freeze-dried, obtains water-soluble graphite
Alkene quanta point material.
The present invention compared with prior art, has following obvious prominent substantive distinguishing features and remarkable advantage:
1. the method for the present invention prepares graphene quantum dot under electric field and ultrasonic field coupling, select cheap and easy to get
Graphite electrode is raw material, using disubstituted imidazole class ionic liquid as electrolyte, at room temperature, in the coupling of electric field and ultrasonic field
Under, water-soluble graphene quantum dot, the method for the present invention green, environmental protection are prepared, simple, safety has large-scale production
Potentiality；
2. the low energy consumption of the method for the present invention energy, expeditiously prepares graphene quantum dot at low cost, by graphite electrode, that is, conduct
Raw material, and reach direct regulation and control carbon source raw material by regulating and controlling electrochemical reaction condition as electrode and be converted into graphene quantum dot
Technique, also directly to open a new way using the development and utilization that inexpensive carbon source prepares graphene.
Detailed description of the invention
Fig. 1 is the TEM image of the graphene quantum dot of one method of embodiment of the present invention preparation.
Fig. 2 is the HRTEM picture of the graphene quantum dot of one method of embodiment of the present invention preparation.
Specific embodiment
Above scheme is described further below in conjunction with specific implementation example, the preferred embodiment of the present invention is described in detail such as
Under:
Embodiment one
In the present embodiment, referring to Fig. 1 and Fig. 2, a kind of to prepare graphene quantum under electric field and ultrasonic field coupling
The method of point, includes the following steps:
A. by -3 methyl imidazolium tetrafluoroborate of 1- ethyl of 4g, i.e. [EMIm] BF4It is dissolved in 100mL deionized water,
Make the electrolyte that concentration is 0.2mol/L；
B. the electrolyte prepared in the step a is placed in electrolytic cell, the graphite flake that two pieces of purity are 99.9% is made
It for electrode, is inserted in parallel into electrolyte, the distance of two graphite electrodes is 3cm, assembles electrochemical reaction appts, and graphite is electric
Pole is as carbon source raw material；
C. the electrolytic cell in the step b is put into ultrasonic pond, according to the ionic liquid used in the step a
Type setting response voltage be 4V, make voltage value control -3 methyl imidazolium tetrafluoroborate ionic liquid of 1- ethyl electrification
Learn in window, setting frequency is 0.2Hz, ultrasonic power 30W, while applying electric field and ultrasonic field to electrolyte, electric field with
Under ultrasonic field coupling, reaction 5h is carried out at room temperature, obtains graphene quantum dot solution；
D. by the step c acquired solution by aperture be that 0.22 μm of microporous barrier is filtered, by filtrate with
The speed of 10000r/min carries out centrifugation 3min, outwells supernatant, then deionized water will be added in the solid content of collection and carries out
Washing, and be repeated as many times, until the pH value of solution after cleaning is neutrality, obtain the dispersion liquid of graphene quantum dot；
E. the dispersion liquid of the gained graphene quantum dot in the step d is freeze-dried, obtains water-soluble graphite
Alkene quanta point material, is stored for future use.Fig. 1 is the TEM image of the graphene quantum dot of preparation, and Fig. 2 is the graphene of preparation
The HRTEM picture of quantum dot.Graphene quantum dot manufactured in the present embodiment is known having a size of 5-10 nanometers, epigranular synthesizes
Quantum dot can be stably dispersed in water, luminescent color or Wavelength tunable.Its biology of graphene quantum dot manufactured in the present embodiment
Compatibility is good, can be equipped with functional group at its edge, have a extensive future in terms of biomarker, luminescent device, solar battery.
The low energy consumption of the present embodiment method energy, expeditiously prepares graphene quantum dot at low cost, by graphite electrode, that is, conduct
Raw material, and reach direct regulation and control carbon source raw material by regulating and controlling electrochemical reaction condition as electrode and be converted into graphene quantum dot
Technique, also directly to open a new way using the development and utilization that inexpensive carbon source prepares graphene.The present embodiment method
Graphene quantum dot is prepared under electric field and ultrasonic field coupling, has selected graphite electrode cheap and easy to get for raw material, with two
Substituted imidazole ionic liquid is that electrolyte under the coupling of electric field and ultrasonic field, has been prepared water-soluble at room temperature
Graphene quantum dot, the present embodiment method green, environmental protection, simple, safety have large-scale production potentiality.
Embodiment two
The present embodiment is basically the same as the first embodiment, and is particular in that:
In the present embodiment, a method of graphene quantum dot being prepared under electric field and ultrasonic field coupling, including
Following steps:
A. by -3 methyl imidazolium tetrafluoroborate of 1- ethyl of 4g, i.e. [EMIm] BF4It is dissolved in 100mL deionized water,
Make the electrolyte that concentration is 0.3mol/L；
B. the electrolyte prepared in the step a is placed in electrolytic cell, the graphite flake that two pieces of purity are 99.9% is made
It for electrode, is inserted in parallel into electrolyte, the distance of two graphite electrodes is 3cm, assembles electrochemical reaction appts, and graphite is electric
Pole is as carbon source raw material；
C. the electrolytic cell in the step b is put into ultrasonic pond, according to the ionic liquid used in the step a
Type setting response voltage be 4V, make voltage value control -3 methyl imidazolium tetrafluoroborate ionic liquid of 1- ethyl electrification
It learns in window, setting frequency is 1Hz, ultrasonic power 90W, while applying electric field and ultrasonic field to electrolyte, in electric field and is surpassed
Under sound field coupling, reaction 8h is carried out at room temperature, obtains graphene quantum dot solution；
D. by the step c acquired solution by aperture be that 0.22 μm of microporous barrier is filtered, by filtrate with
The speed of 15000r/min carries out centrifugation 3min, outwells supernatant, then deionized water will be added in the solid content of collection and carries out
Washing, and be repeated as many times, until the pH value of solution after cleaning is neutrality, obtain the dispersion liquid of graphene quantum dot；
E. the dispersion liquid of the gained graphene quantum dot in the step d is freeze-dried, obtains water-soluble graphite
Alkene quanta point material, is stored for future use.Graphene quantum dot manufactured in the present embodiment is having a size of 5-10 nanometers, epigranular,
The low energy consumption of the present embodiment method energy, expeditiously prepares graphene quantum dot at low cost, that is, regard graphite electrode as raw material, again
Reach direct regulation and control carbon source raw material by regulation electrochemical reaction condition as electrode and be converted into graphene quantum dot technique,
Directly to open a new way using the development and utilization that inexpensive carbon source prepares graphene.The present embodiment method in electric field and
Graphene quantum dot is prepared under ultrasonic field coupling, has selected graphite electrode cheap and easy to get for raw material, with disubstituted imidazole
Class ionic liquid is that electrolyte under the coupling of electric field and ultrasonic field, has prepared water-soluble graphene amount at room temperature
Sub-, the present embodiment method green, environmental protection, simple, safety have large-scale production potentiality.
Embodiment three
The present embodiment is substantially the same as in the previous example, and is particular in that:
In the present embodiment, a method of graphene quantum dot being prepared under electric field and ultrasonic field coupling, including
Following steps:
A. by -3 methyl imidazolium tetrafluoroborate of 1- ethyl of 4g, i.e. [EMIm] BF4It is dissolved in 100mL deionized water,
Make the electrolyte that concentration is 0.1mol/L；
B. the electrolyte prepared in the step a is placed in electrolytic cell, the graphite flake that two pieces of purity are 99.9% is made
It for electrode, is inserted in parallel into electrolyte, the distance of two graphite electrodes is 3cm, assembles electrochemical reaction appts, and graphite is electric
Pole is as carbon source raw material；
C. the electrolytic cell in the step b is put into ultrasonic pond, according to the ionic liquid used in the step a
Type setting response voltage be 4V, make voltage value control -3 methyl imidazolium tetrafluoroborate ionic liquid of 1- ethyl electrification
Learn in window, setting frequency is 0.05Hz, ultrasonic power 60W, while applying electric field and ultrasonic field to electrolyte, electric field with
Under ultrasonic field coupling, reaction 8h is carried out at room temperature, obtains graphene quantum dot solution；
D. by the step c acquired solution by aperture be that 0.22 μm of microporous barrier is filtered, by filtrate with
The speed of 15000r/min carries out centrifugation 5min, outwells supernatant, then deionized water will be added in the solid content of collection and carries out
Washing, and be repeated as many times, until the pH value of solution after cleaning is neutrality, obtain the dispersion liquid of graphene quantum dot；
E. the dispersion liquid of the gained graphene quantum dot in the step d is freeze-dried, obtains water-soluble graphite
Alkene quanta point material, is stored for future use.Graphene quantum dot manufactured in the present embodiment is having a size of 5-10 nanometers, epigranular,
The low energy consumption of the present embodiment method energy, expeditiously prepares graphene quantum dot at low cost, that is, regard graphite electrode as raw material, again
Reach direct regulation and control carbon source raw material by regulation electrochemical reaction condition as electrode and be converted into graphene quantum dot technique,
Directly to open a new way using the development and utilization that inexpensive carbon source prepares graphene.The present embodiment method in electric field and
Graphene quantum dot is prepared under ultrasonic field coupling, has selected graphite electrode cheap and easy to get for raw material, with disubstituted imidazole
Class ionic liquid is that electrolyte under the coupling of electric field and ultrasonic field, has prepared water-soluble graphene amount at room temperature
Sub-, the present embodiment method green, environmental protection, simple, safety have large-scale production potentiality.
Combination attached drawing of the embodiment of the present invention is illustrated above, but the present invention is not limited to the above embodiments, it can be with
The purpose of innovation and creation according to the present invention makes a variety of variations, under the Spirit Essence and principle of all technical solutions according to the present invention
Change, modification, substitution, combination or the simplification made, should be equivalent substitute mode, as long as meeting goal of the invention of the invention,
The technical principle and hair of the method for graphene quantum dot are prepared under electric field and ultrasonic field coupling without departing from the present invention
Bright design, belongs to protection scope of the present invention.
Claims (4)
1. a kind of method for preparing graphene quantum dot under electric field and ultrasonic field coupling, which is characterized in that including as follows
Step:
A. disubstituted imidazole class ionic liquid is mixed with deionized water, compound concentration is the electrolyte of 0.1~0.3mol/L；
B. the electrolyte prepared in the step a is placed in electrolytic cell, with two graphite electrodes, is inserted in parallel into electrolyte
In, electrochemical reaction appts are assembled, and using graphite electrode as carbon source raw material；
C. the electrolytic cell in the step b is put into ultrasonic pond, response voltage, voltage is arranged according to the type of ionic liquid
In the electrochemical window of the used ionic liquid of step a, setting frequency is 0.05~1Hz for value control, and ultrasonic power is
30~90W, while 5~10h of reaction is carried out under electric field and ultrasonic field coupling to electrolyte application electric field and ultrasonic field,
Obtain graphene quantum dot solution；
D. by the step c acquired solution be filtered not higher than 0.22 μm of microporous barrier by aperture, by filtrate with
The speed of 10000~15000r/min carries out 3~5min of centrifugation, outwells supernatant, then will be added and goes in the solid content of collection
Ionized water is washed, and is repeated as many times, until the pH value of solution after cleaning is neutrality, obtains the dispersion liquid of graphene quantum dot；
E. the dispersion liquid of the gained graphene quantum dot in the step d is freeze-dried, obtains water-soluble graphene amount
Son point material.
2. the method for preparing graphene quantum dot under electric field and ultrasonic field coupling according to claim 1, feature
It is: in the step b, makes the distance of two graphite electrodes not less than 3cm.
3. the method for preparing graphene quantum dot under electric field and ultrasonic field coupling according to claim 1, feature
Be: in the step a, the disubstituted imidazole class ionic liquid uses -3 methyl imidazolium tetrafluoroborate of 1- ethyl.
4. the method for preparing graphene quantum dot under electric field and ultrasonic field coupling according to claim 1, feature
It is: in the step c, under electric field and ultrasonic field coupling, is reacted at room temperature, prepare graphene amount
Son point solution.
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