CN108751167A - A kind of graphene solution preparation method - Google Patents
A kind of graphene solution preparation method Download PDFInfo
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- CN108751167A CN108751167A CN201810451678.XA CN201810451678A CN108751167A CN 108751167 A CN108751167 A CN 108751167A CN 201810451678 A CN201810451678 A CN 201810451678A CN 108751167 A CN108751167 A CN 108751167A
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- graphene
- solution
- sheet metal
- metal
- reaction kettle
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/184—Preparation
Abstract
The invention discloses a kind of graphene solution preparation methods, graphite is dissolved into liquid, sheet metal is impregnated under high temperature environment using liquid, improve the carbon content in sheet metal, C-H bond cleavage in liquid is immersed in metal and entrance, in metal graphene solid is generated in metal surface by the moment of high temperature to low temperature, graphene suspension is set to be in neutrality using deionized water, graphene is set to be more evenly distributed in the solution using centrifugal treating, utilize vacuum spray drying, it is dried under the situation for not changing graphene characteristic, obtain the graphene particles of pure matter, to be prepared into pure graphene solution.
Description
Technical field
The present invention relates to a kind of field of graphene, specifically a kind of graphene solution preparation method.
Background technology
The arrangement mode of graphene internal carbon as graphite monoatomic layer with sp2 hybridized orbit bondings, and just like
Under feature：Carbon atom has 4 valence electrons, wherein 3 are electronically generated sp2 keys, i.e., each carbon atom contributes one to be located at pz
Non- bonding electrons on track, pz tracks and the plane of neighbour's atom can form pi bond at vertical direction, and the pi bond newly formed is in half
Fill up state.Research confirms that the ligancy of carbon atom is 3 in graphene, the bond distance between each two adjacent carbon atom is 1.42 ×
10-10 meters, the angle between key and key is 120 °.In addition to σ keys and other carbon atom chains are connected into the cellular stratiform knot of hexagonal ring
Outside structure, the pz tracks perpendicular to layer plane of each carbon atom can form polyatomic big pi bond through holostrome (with phenyl ring class
Like), thus there is excellent conduction and optical property.
Graphene because of its excellent optics, electricity, mechanical characteristic, materialogy, micro-nano technology, the energy, biomedicine and
Drug delivery etc. is with important application prospects, it is considered to be a kind of future revolutionary material.Manchester, England is big
Physicist An Deliegaimu and Constantine's Nuo Woxiao loves are learned, is isolated from graphite with micromechanics stripping method success
Graphene, therefore Nobel Prize in physics in 2010 is obtained jointly.
But the purity that uses on the market it is high graphene cost of manufacture it is high, and its is pure for the graphene that low-cost production comes out
Degree cannot be guaranteed that the purity liquid of the graphene solution obtained from can not ensure, influence its quality.
Invention content
It is mentioned above in the background art to solve the purpose of the present invention is to provide a kind of graphene solution preparation method
Problem.
To achieve the above object, the present invention provides the following technical solutions：
A kind of graphene solution preparation method, specific preparation process are as follows：
S1, chlorosulfonic acid solution is imported into receptacle, takes appropriate graphite, be conducted into inside chlorosulfonic acid solution, ceaselessly
Stirring later concentrates solution until graphite is dissolved in inside chlorosulfonic acid solution, is then poured into inside reaction kettle,
It is put into suitable sheet metal inside to reaction kettle, is then passed through protective gas to reaction kettle the inside, the protective gas is argon
Gas and helium control the temperature rise inside reaction kettle to 900-1200 degrees Celsius, and sheet metal impregnates one section inside solution
Time is then shut off reaction kettle and takes out sheet metal until the carbon inside solution enters inside sheet metal, quickly will
It is put into inside freezing chamber, and for sheet metal inside freezing chamber, the carbon that ontology immerses is formed on its surface a layer graphene, will
Graphene, which is wiped off, pours into receptacle, and the soak in reaction kettle is taken out and stands 60-80 minutes, by upper layer graphene suspended matter
It takes out；
S2, pure water is imported to receptacle, forms graphene suspension, to graphene suspension the inside addition step S1
In graphene suspended matter obtained, stir evenly, the liquid of receptacle cleaned with deionized water, until during solution is in
Property, then solution is ultrasonically treated, obtains uniform solution, solution is put into inside centrifuge carries out at centrifugation later
Reason, later washs solution, is conducted into vacuum spray dehydrator and processing is dried, graphene particles, then will
Graphene particles are dissolved in pure water, stir evenly and graphene solution is made.
As a further solution of the present invention：The rotating speed stirred when graphite dissolves in the step S1 is 15-20 revs/min.
As a further solution of the present invention：Sheet metal is the transition such as Fe, Ru, Co, Rh, Ir gold in the step S1
Belong to.
As a further solution of the present invention：Sheet metal impregnates 30-35 minutes inside solution in the step S1.
As a further solution of the present invention：Temperature control in the step S1 inside freezing chamber is Celsius in subzero 1-2
Degree.
As a further solution of the present invention：Graphene suspension is cleaned 2-3 times with deionized water in the step S2.
As a further solution of the present invention：The time being ultrasonically treated in the step S2 is 20-30 minutes.
As further scheme of the invention：The rotating speed of centrifuge is 800-1200 revs/min in the step S2, centrifugation
Time is 40-50 minutes.
Compared with prior art, the beneficial effects of the invention are as follows：Graphite is dissolved into liquid, using liquid in hot environment
Under sheet metal is impregnated, improve the carbon content in sheet metal, it is in metal and enter and immerse C-H bond cleavage in liquid,
Graphene solid is generated in metal surface by the moment of high temperature to low temperature in metal, makes the graphene suspension be in using deionized water
Neutrality makes graphene be more evenly distributed in the solution using centrifugal treating, using vacuum spray drying, is not changing graphene spy
It is dried under the situation of property, the graphene particles of pure matter are obtained, to be prepared into pure graphene solution.
Specific implementation mode
Below in conjunction with the embodiment of the present invention, technical scheme in the embodiment of the invention is clearly and completely described,
Obviously, described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.Based in the present invention
Embodiment, every other embodiment obtained by those of ordinary skill in the art without making creative efforts, all
Belong to the scope of protection of the invention.
In the embodiment of the present invention, a kind of graphene solution preparation method, specific preparation process is as follows：
S1, chlorosulfonic acid solution is imported into receptacle, takes appropriate graphite, be conducted into inside chlorosulfonic acid solution, ceaselessly
The rotating speed of stirring, stirring is 15-20 revs/min, until graphite is dissolved in inside chlorosulfonic acid solution, is concentrated later to solution,
Then be poured into inside reaction kettle, to reaction kettle inside be put into suitable sheet metal, the sheet metal is Fe, Ru, Co,
Then the transition metal such as Rh, Ir are passed through protective gas to reaction kettle the inside, the protective gas is argon gas and helium, and control is anti-
Answer the temperature rise inside kettle to 900-1200 degrees Celsius, sheet metal impregnates 30-35 minutes inside solution, until in solution
The carbon in face enters inside sheet metal, is then shut off reaction kettle and takes out sheet metal, quickly puts it into freezing chamber
Face, the temperature control inside freezing chamber is at subzero 1-2 degrees Celsius, and inside freezing chamber, the carbon that ontology immerses exists sheet metal
Its surface forms a layer graphene, and graphene is wiped off and pours into receptacle, and the soak in reaction kettle is taken out and stands 60-80
Minute, upper layer graphene suspended matter is taken out, sheet metal is impregnated under high temperature environment using liquid, improves metal foil
Carbon content in piece, it is in metal and enter and immerse C-H bond cleavage in liquid, in metal by the moment of high temperature to low temperature in metal
Surface Creation graphene solid；
S2, pure water is imported to receptacle, forms graphene suspension, to graphene suspension the inside addition step S1
In graphene suspended matter obtained, stir evenly, the liquid of receptacle cleaned with deionized water, clean 2-3 times, directly
It being in neutrality to solution, then solution is ultrasonically treated, the time of supersound process is 20-30 minutes, obtains uniform solution,
Solution is put into inside centrifuge later and carries out centrifugal treating, the rotating speed of centrifuge is 800-1200 revs/min, and centrifugation time is
40-50 minutes, solution is washed later, is conducted into vacuum spray dehydrator and processing is dried, graphene particles,
Then graphene particles are dissolved in pure water, stir evenly and graphene solution is made, using vacuum spray drying, do not changed
It is dried under the situation of graphene characteristic, obtains the graphene particles of pure matter, to which the graphene for being prepared into pure is molten
Liquid.
The present invention operation principle be：Graphite is dissolved into liquid, using liquid under high temperature environment to sheet metal into
Row impregnates, and improves the carbon content in sheet metal, in metal and enter and immerse C-H bond cleavage in liquid, metal by high temperature extremely
The moment of low temperature generates graphene solid in metal surface, so that graphene suspension is in neutrality using deionized water, utilizes centrifugation
Processing makes graphene be more evenly distributed in the solution, right under the situation for not changing graphene characteristic using vacuum spray drying
It is dried, and obtains the graphene particles of pure matter, to be prepared into pure graphene solution.
It is obvious to a person skilled in the art that invention is not limited to the details of the above exemplary embodiments, Er Qie
In the case of without departing substantially from spirit or essential attributes of the invention, the present invention can be realized in other specific forms.Therefore, no matter
From the point of view of which point, the present embodiments are to be considered as illustrative and not restrictive, and the scope of the present invention is by appended power
Profit requires rather than above description limits, it is intended that all by what is fallen within the meaning and scope of the equivalent requirements of the claims
Variation is included within the present invention.
In addition, it should be understood that although this specification is described in terms of embodiments, but not each embodiment is only wrapped
Containing an independent technical solution, this description of the specification is merely for the sake of clarity, and those skilled in the art should
It considers the specification as a whole, the technical solutions in the various embodiments may also be suitably combined, forms those skilled in the art
The other embodiment being appreciated that.
Claims (8)
1. a kind of graphene solution preparation method, which is characterized in that its specific preparation process is as follows：
S1, chlorosulfonic acid solution is imported into receptacle, takes appropriate graphite, be conducted into inside chlorosulfonic acid solution, ceaselessly stir,
Until graphite is dissolved in inside chlorosulfonic acid solution, solution is concentrated later, is then poured into inside reaction kettle, to reaction
It is put into suitable sheet metal inside kettle, is then passed through protective gas to reaction kettle the inside, the protective gas is argon gas and helium
Gas controls the temperature rise inside reaction kettle to 900-1200 degrees Celsius, and sheet metal is soaked for a period of time inside solution, directly
Carbon inside to solution enters inside sheet metal, is then shut off reaction kettle and takes out sheet metal, quickly puts it into
Inside freezing chamber, sheet metal is inside freezing chamber, and the carbon that ontology immerses is formed on its surface a layer graphene, by graphene
It wipes off and pours into receptacle, the soak in reaction kettle is taken out and stands 60-80 minutes, upper layer graphene suspended matter is taken out；
S2, pure water is imported to receptacle, forms graphene suspension, made into graphene suspension the inside addition step S1
The graphene suspended matter obtained, stirs evenly, is cleaned to the liquid of receptacle with deionized water, until solution is in neutrality,
Then solution is ultrasonically treated, obtains uniform solution, solution is put into inside centrifuge carry out centrifugal treating later, it
Solution is washed afterwards, is conducted into vacuum spray dehydrator and processing is dried, graphene particles, then by graphene
Particle is dissolved in pure water, stirs evenly and graphene solution is made.
2. a kind of graphene solution preparation method according to claim 1, which is characterized in that graphite is molten in the step S1
The rotating speed stirred when solution is 15-20 revs/min.
3. a kind of graphene solution preparation method according to claim 1, which is characterized in that metal foil in the step S1
Piece is the transition metal such as Fe, Ru, Co, Rh, Ir.
4. a kind of graphene solution preparation method according to claim 1, which is characterized in that metal foil in the step S1
Piece impregnates 30-35 minutes inside solution.
5. a kind of graphene solution preparation method according to claim 1, which is characterized in that freezing chamber in the step S1
The temperature of the inside is controlled at subzero 1-2 degrees Celsius.
6. a kind of graphene solution preparation method according to claim 1, which is characterized in that spent in the step S2 from
Sub- water cleans graphene suspension 2-3 times.
7. a kind of graphene solution preparation method according to claim 1, which is characterized in that in the step S2 at ultrasound
The time of reason is 20-30 minutes.
8. a kind of graphene solution preparation method according to claim 1, which is characterized in that centrifuge in the step S2
Rotating speed be 800-1200 revs/min, centrifugation time be 40-50 minutes.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109455709A (en) * | 2018-12-25 | 2019-03-12 | 中国科学院电工研究所 | A kind of graphene powder material and preparation method thereof |
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| CN102627272A (en) * | 2012-04-12 | 2012-08-08 | 中国科学院长春应用化学研究所 | Method for preparing less layer graphene sheet |
| CN102627274A (en) * | 2012-04-23 | 2012-08-08 | 中国科学院上海微***与信息技术研究所 | Method for preparing graphene |
| CN102627275A (en) * | 2012-04-28 | 2012-08-08 | 郑州大学 | Method for preparing graphene by melting carbon-containing alloy to separate out carbon in solidification process |
| CN102627273A (en) * | 2012-04-19 | 2012-08-08 | 常州第六元素材料科技股份有限公司 | Purifying process for graphene material of energy storing device |
-
2018
- 2018-05-12 CN CN201810451678.XA patent/CN108751167A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102627272A (en) * | 2012-04-12 | 2012-08-08 | 中国科学院长春应用化学研究所 | Method for preparing less layer graphene sheet |
| CN102627273A (en) * | 2012-04-19 | 2012-08-08 | 常州第六元素材料科技股份有限公司 | Purifying process for graphene material of energy storing device |
| CN102627274A (en) * | 2012-04-23 | 2012-08-08 | 中国科学院上海微***与信息技术研究所 | Method for preparing graphene |
| CN102627275A (en) * | 2012-04-28 | 2012-08-08 | 郑州大学 | Method for preparing graphene by melting carbon-containing alloy to separate out carbon in solidification process |
Non-Patent Citations (2)
| Title |
|---|
| NATNAEL BEHABTU等: "Spontaneous high-concentration dispersions and liquid crystals of graphene", 《NATURE NANOTECHNOLOGY》 * |
| WENCHENG DU等: "From graphite to graphene: direct liquid-phase exfoliation of graphite to produce single- and few-ayered", 《JOURNAL OF MATERIALS CHEMISTRY A》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109455709A (en) * | 2018-12-25 | 2019-03-12 | 中国科学院电工研究所 | A kind of graphene powder material and preparation method thereof |
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