CN106629673A - Preparation method for graphene oxide - Google Patents
Preparation method for graphene oxide Download PDFInfo
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- CN106629673A CN106629673A CN201610822040.3A CN201610822040A CN106629673A CN 106629673 A CN106629673 A CN 106629673A CN 201610822040 A CN201610822040 A CN 201610822040A CN 106629673 A CN106629673 A CN 106629673A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
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Abstract
The invention especially relates to a preparation method for graphene oxide, belonging to the technical field of graphene preparation. The preparation method comprises the following steps: (1) with common graphite as a raw material, preparing graphite suspension containing thin graphite flakes by using a liquid-phase peeling method; (2) carrying out filtering and drying obtain graphite sheet powder; (3) adding an oxidizing agent and carrying out an oxidation reaction; (4) forming graphite oxide at 20 to 40 DEG C by using an oxidation ice-splashing method; and (5) cleaning and drying the graphite oxide, adding deionized water or an organic solvent and carrying out ultrasonic treatment so as to obtain graphene oxide dispersion liquid containing graphene oxide. According to the invention, ultrasonic concussion is carried out peel graphite and then oxidation is carried out so as to prepare graphene oxide, and the prepared graphene oxide can be uniformly dispersed in water, an acidic solution, an alkaline solution or an organic solution to form uniformly dispersed graphene oxide. The method provided by the invention has the advantages of simple process, high success rate, easily controllable operation conditions, etc.
Description
Technical field
The invention belongs to technical field of graphene preparation, more particularly to a kind of preparation method of graphene oxide.
Background technology
Graphene (Graphene) be it is a kind of by carbon atom with sp2 hybridized orbits constitute hexangle type in honeycomb lattice plane
Film, the two-dimensional material of only one of which carbon atom thickness.Graphene is considered as always hypothetical structure, it is impossible to individually stable
Exist, until 2004, Univ Manchester UK physicist An Deliehaimu and Constantine's Nuo Woxiao loves, into
Work(ground is just separated for the first time using micromechanics stripping method in an experiment from graphite and observes single-layer graphene, so as to confirm
It can be with individualism, and two people also because of " in the initiative experiment of two-dimensional graphene material ", obtain Nobel in 2010 jointly
PHYSICS.
It is but also most hard nano material that Graphene is currently world most thin, and it is almost fully transparent, is only absorbed
2.3% light；Thermal conductivity factor is up to 5300W/mK, and higher than CNT and diamond, its electron mobility exceedes under normal temperature
15000cm2/ Vs, but it is higher than CNT or silicon crystal, and resistivity about 10-6Ω cm, it is lower than copper or silver, it is mesh
The minimum material of resistivity on previous existence.Because its resistivity is extremely low, the speed that electronics runs is exceedingly fast, therefore is expected to can be used to send out
Put on display thinner, conductive speed a new generation's electronic component or transistor faster.Because Graphene is substantially a kind of transparent, good
Conductor, also be adapted for for manufacturing transparent touch screen, even tabula rasa, solar cell.
Graphene oxide is product of the powdered graphite after chemical oxidation and delamination, and graphene oxide is single atom
Layer, can on lateral dimension from tens nanometers to some tens of pm, therefore, the general chemistry of its construct trans and material science
Typical size.Graphene oxide can be considered a kind of flexible material of non-traditional form, with polymer, colloid, film
Characteristic.Because graphene oxide has derivative carboxyl at lamella edge, in the plane with phenolic hydroxyl group and epoxide group, conjugation
Network receives serious functionalization, and graphene oxide has regulatable surface-active, and electrical and optical characteristics, is to prepare graphite
Important intermediate compound during alkene compound and graphene functionalized.It is extensive that graphene oxide is prepared with graphite powder
The starting point of Graphene is prepared, is also to realize one of effective ways that Graphene is prepared in a large number.
At present, relatively conventional graphene oxide preparation method mainly has：Brodie methods, Staudenmaier methods,
Hummers methods.
Chinese patent application CN101817516A is peeled off to be separated after carbon materials using solid particle Aided Machine and obtains stone
Black alkene or graphene oxide, but be not using liquid phase householder method and removing solid particle difficulty.
Graphite powder, sodium nitrate low-temperature oxidation in concentrated sulfuric acid is subsequently adding height by Chinese patent application CN105399084A
Potassium manganate further aoxidizes intercalation under middle temperature, and finally at high temperature reaction obtains graphene oxide, and the method is needed in high temperature
Lower reaction, increased control difficulty.
Chinese patent application CN104876219A under 10-30 DEG C of normal temperature, is mixed based on Hummers methods to graphite oxide
Hydrogen peroxide solution is added in liquid, graphene oxide water solution is obtained under ul-trasonic irradiation, but the graphite that the method is first carried out
Oxidation step, thus it is higher to the quality requirements of graphite raw material, increased the manufacturing cost of graphene oxide.
Although in actual mechanical process, said method can successfully prepare graphene oxide, said method
It is higher for the requirement of raw graphite, generally require using the crystalline flake graphite raw material for being easier to oxidation reaction, and if
Using thicker, larger graphite powder, it is difficult to make the graphene oxide of high-quality, therefore being manufactured into for graphene oxide is improve
This.In addition, above-mentioned preparation method is in graphite oxide step is prepared, generally require to be higher than to carry out at a temperature of room temperature, and need
Strict controlling reaction temperature, once temperature control is bad, may result in preparation failure.
The content of the invention
It is an object of the invention to provide a kind of preparation method of improved graphene oxide, can use the larger graphite of particle
Powder, and high-temperature heating need not be carried out in graphite oxide step is prepared, it is easy to prepare.
To achieve these goals, the invention provides following technical scheme：
The present invention provides a kind of preparation method of graphene oxide, comprises the following steps：
(1) graphite suspension is prepared：With common graphite powder as raw material, it is obtained using liquid phase stripping method and contains thin graphite flake layer
Graphite suspension；
(2) graphite flake powder is prepared：To graphite suspension obtained in step (1), filtered and be dried, obtained graphite
Flake powder；
(3) intercalation：Solvent is added in graphite flake powder obtained in step (2), intercalation is carried out；
(4) graphite oxide is prepared：To step (3) resulting solution, ice method is sprinkled by oxidation oxidation is formed at 20 DEG C -40 DEG C
Graphite；
(5) clean and ultrasonically treated：Graphite oxide obtained in step (4) is cleaned and is dried；Be subsequently adding from
Sub- water or organic solvent, and carry out ultrasonically treated, obtain the graphene oxide dispersion containing graphene oxide.
In the step (1), the common graphite powder is selected from crystalline graphite powder, expansible graphite powder or microcrystal graphite
Powder.
In the step (1), the liquid phase stripping method detailed process is：Common graphite powder, institute are added in liquid solution
The 0.1-2% of the weight for liquid solution weight of common graphite powder is stated, at 20 DEG C -50 DEG C of temperature and airtight condition, with big
In being shaken or being ground equal to the ultrasonic wave of 80 watts of power, concussion or milling time are 1-12 hours.
The liquid solution is selected from one of following mixed liquor：
Deionized water and acetone mixture, wherein acetone are 70-90wt%；Or
Acetone and alcohol mixeding liquid, wherein acetone are 70-90wt%；Or
Acetone and N- methyl-prop network alkanone mixed liquors, wherein acetone are 10-30wt%.
In the filtration step of the step (2), using ordinary filter paper or membrane filtration, the ordinary filter paper is experiment
Qualitative or quantitative filter paper.
In the drying steps of the step (2), baking temperature is 40 DEG C -90 DEG C, and the time is 6-12 hours.
In the step (3), graphite flake powder and solvent mixture are placed in ice bath with magnetic agitation 2-4 hour,
Keeping temperature is between 0 DEG C -5 DEG C, graphite flake powder is sufficiently mixed with solvent.
In the step (3), the intercalation solvent is the combination of sodium nitrate and the concentrated sulfuric acid, or for red fuming nitric acid (RFNA) and dense
The combination of sulfuric acid.
Graphite flake powder is 2 with the part by weight of sodium nitrate and the concentrated sulfuric acid：1：80-100；Graphite flake powder and dense nitre
The part by weight of acid and the concentrated sulfuric acid is 1：15-20：55-70.
In the step (4), the oxidation is sprinkled ice method detailed process and is：
Under condition of ice bath, continue whipping step (3) resulting solution, be slowly added to potassium permanganate, the potassium permanganate with
The weight ratio of the common graphite powder is 3：1, during potassium permanganate is added, solution temperature is not higher than 10 DEG C；Treat permanganic acid
Potassium starts timing after all adding, and stirring reaction 0.5-2 hour is continued under ice bath；Now, solution is blackish green；By beaker
In moving to 20 DEG C of -40 DEG C of tepidariums, stirring reaction 6-8 hour；
Then, potassium permanganate is disposably added, the potassium permanganate is 3 with the weight ratio of the common graphite powder：1,
8-12 hours are stirred in 20 DEG C of -40 DEG C of tepidariums；Product is cooled to after room temperature, is sprinkled containing 5-30% hydrogen peroxide
On the ice cube of the aqueous solution, and stir, in whipping process, then hydrogenperoxide steam generator is added dropwise, solution can become bright orange from reddish brown
Color solution, obtains graphite oxide in ie in solution.
In the step (5), using deionized water cleaning operation is carried out.
The organic solvent is N- methyl-prop network alkanones NMP, dimethylformamide DMF or dimethyl sulfoxide (DMSO) DMSO.
Compared with prior art, the beneficial effects of the present invention is：
, for being prepared during graphene oxide using chemical oxidization method at present, powdered graphite is thicker, prepares for the present invention
Journey temperature control is difficult, is easier to the technical problem that failure occurs, on the premise of advance liquid phase peels off graphite, it is to avoid to product
High-temperature heating is carried out, reduces preparing difficulty, improve success rate.There is the method process is simple, low cost, operating condition to be easy to control
Processed the advantages of.The present invention prepares graphene oxide at 20-40 DEG C using liquid phase lift-off technology assistant reinforcement, eliminates
High-temperature step in Hummers methods, improves production graphene oxide yield rate and quality.
Description of the drawings
Fig. 1 present invention prepares the flow chart of the method for graphene oxide；
The Raman spectrogram of the graphene oxide that Fig. 2 is prepared using crystalline graphite powder
The transmission electron microscope shape appearance figure of the graphene oxide that Fig. 3 is prepared using crystalline graphite powder；
The transmission electron microscope shape appearance figure of the graphene oxide that Fig. 4 is prepared using expansible graphite powder；
The transmission electron microscope shape appearance figure of the graphene oxide that Fig. 5 is prepared using microlite ink powder.
Specific embodiment
The present invention is further described with reference to embodiment.
A kind of preparation method of graphene oxide of the present invention, comprises the following steps：
(1) graphite suspension is prepared：With common graphite powder as raw material, it is obtained using liquid phase stripping method and contains thin graphite flake layer
Graphite suspension.
The common graphite powder is selected from crystalline graphite powder, expansible graphite powder or microcrystal graphite powder.
The liquid phase stripping method detailed process is：Common graphite powder is added in liquid solution, common graphite powder is added
Weight is the 0.1-2% of liquid solution weight.Preferably, the weight of common graphite powder is the 0.5-2% of liquid solution weight.
At 20 DEG C -50 DEG C of temperature and airtight condition, shaken or ground with the ultrasonic wave more than or equal to 80 watts of power, concussion or
Milling time is 1-12 hours.
The liquid solution is the mixed solution for meeting the theoretical any two of Graphene Hansen solubility parameters, is preferably gone
The mixed liquor of ionized water and acetone, acetone and ethanol, acetone and N- methyl-props network alkanone (NMP).
Deionized water and acetone mixture, wherein acetone are 70-90wt%；Or
Acetone and alcohol mixeding liquid, wherein acetone are 70-90wt%；Or
Acetone and N- methyl-prop network alkanone mixed liquors, wherein acetone are 10-30wt%.
(2) graphite flake powder is prepared：To graphite suspension obtained in step (1), filtered and be dried, obtained graphite
Flake powder.
Using ordinary filter paper, the qualitative or quantitative filter paper of such as experiment is filtered, or is entered using filter membrane such as miillpore filter
Row is filtered.
Baking temperature is 40 DEG C -90 DEG C, and the time is 6-12 hours.
(3) intercalation：Solvent is added in graphite flake powder obtained in step (2), intercalation is carried out；By graphite
Flake powder and solvent mixture are placed in ice bath with magnetic agitation 2-4 hour, are maintained the temperature between 0 DEG C -5 DEG C, make graphite
Flake powder is sufficiently mixed with solvent.
The intercalation solvent is the combination of sodium nitrate and the concentrated sulfuric acid, or for the combination of red fuming nitric acid (RFNA) and the concentrated sulfuric acid；
Graphite flake powder is 2 with the part by weight of sodium nitrate and the concentrated sulfuric acid：1：80-100, graphite flake powder and dense nitre
The part by weight of acid and the concentrated sulfuric acid is 1：15-20：55-70.
(4) graphite oxide is prepared：To step (3) resulting solution, ice method is sprinkled by oxidation oxidation stone is formed at 20-40 DEG C
Ink；
Oxidation is sprinkled ice method and forms graphene oxide at 20 DEG C -40 DEG C, eliminates the hot stage in conventional H ummers method
(being higher than 80 DEG C), only need to be by simply adding twice a potassium permanganate.
Ice method detailed process is sprinkled in the oxidation：
Under condition of ice bath, continue whipping step (3) resulting solution, be slowly added to potassium permanganate, the potassium permanganate with
The weight ratio of the common graphite powder is 3：1, it is ensured that during potassium permanganate is added, solution temperature is not higher than 10 DEG C；Treat height
Potassium manganate starts timing after all adding, and stirring reaction 0.5-2 hour is continued under ice bath.Now, solution is blackish green；Will
Beaker is moved in 20 DEG C of -40 DEG C of tepidariums, stirring reaction 6-8 hour.
Then, potassium permanganate is disposably added, the potassium permanganate, the weight of the potassium permanganate and the common graphite powder
Amount is than being 3：1,8-12 hours are stirred in 20 DEG C of -40 DEG C of tepidariums.Product is cooled to after room temperature, is sprinkled and is being contained 5-
On the ice cube of 30% aqueous hydrogen peroxide solution.In whipping process, then hydrogenperoxide steam generator is added dropwise, solution can become from reddish brown
Bright yellow solution, obtains graphite oxide in ie in solution.
(5) clean and ultrasonically treated：Graphite oxide obtained in step (4) is cleaned and is dried；Be subsequently adding from
Sub- water or organic solvent, and carry out ultrasonically treated, obtain the graphene oxide dispersion containing graphene oxide.
In step (5), using deionized water cleaning operation is carried out.
The organic solvent is N- methyl-props network alkanone (NMP), dimethylformamide (DMF), dimethyl sulfoxide (DMSO) (DMSO)
Deng.
Embodiment 1
With crystalline graphite powder as primary raw material, choose acetone and water is prepared and peels off graphite powder.160mL acetone is taken, 40mL goes
Ionized water.2g crystalline graphite powders are taken, in adding mixed liquor, the lower 80 watts of power ultrasonics concussion of airtight condition, keeping temperature is not higher than
50 DEG C, the concussion time is 6 hours.
After the completion of, filter paper is filtered, then is dried 6 hours at 40 DEG C, obtains graphite flake powder.
1g graphite flake powder is taken, adds 0.5g sodium nitrate, the 43g concentrated sulfuric acids to be placed in ice bath little with magnetic agitation 3
When, keeping temperature is 0 DEG C.
Under condition of ice bath and continue agitating solution, be slowly added to 3g potassium permanganate, it is ensured that add potassium permanganate mistake
Cheng Zhong, solution temperature is not higher than 10 DEG C.Treat that potassium permanganate starts timing after all adding, stirring reaction 2 is continued under ice bath
Hour.Now, solution is blackish green.Beaker is moved in 20 DEG C of tepidariums, stirring reaction 7 hours.Again property adds 3g high
Potassium manganate, is stirred for 12 hours in 20 DEG C of tepidarium.Product is cooled to after room temperature, is sprinkled containing 30% hydrogen peroxide
On the ice cube of the aqueous solution.In whipping process, then hydrogenperoxide steam generator is added dropwise, solution can become bright yellow solution from reddish brown,
Graphite oxide is obtained in ie in solution.
By being cleaned multiple times, after collecting solid, it is dried 12 hours below 60 DEG C, obtains graphene oxide powder.Weigh
Certain powder adds deionized water, ultrasonic vibration, you can obtain graphene oxide dispersion.
Embodiment 2
With expansible graphite powder as primary raw material, prepared with acetone and ethanol and peel off graphite powder.180mL acetone, 20mL second
Alcohol, 1g expansible graphite powder is well mixed rear mixed liquor ultrasonic vibration in confined conditions, and keeping temperature is not higher than 50 DEG C, shake
The time is swung for 6 hours.
After the completion of, filter paper is filtered, then is dried 6 hours at 50 DEG C, obtains graphite flake powder.
The 60g concentrated sulfuric acids are added in 1g graphite flake powder, is placed in ice bath with magnetic agitation 3 hours, slow drop
Enter 18g red fuming nitric acid (RFNA)s, keeping temperature is 4 DEG C, is stirred 40 minutes.
Under condition of ice bath and continue agitating solution, be slowly added to 3g potassium permanganate, it is ensured that add potassium permanganate mistake
Cheng Zhong, solution temperature is not above 10 DEG C.Treat that potassium permanganate starts timing after all adding, stirring reaction is continued under ice bath
2 hours.Beaker is moved in 31 DEG C of tepidariums, stirring reaction 7 hours.Again property adds 3g potassium permanganate, in 31 DEG C of warm water
12 hours are stirred in bath.Product is cooled to after room temperature, is sprinkled on the ice cube containing 10% aqueous hydrogen peroxide solution.Stir
During mixing, then hydrogenperoxide steam generator is added dropwise, solution can become bright yellow solution from reddish brown, obtains aoxidizing stone in ie in solution
Ink.
By being cleaned multiple times, after collecting solid, it is dried 12 hours below 60 DEG C, this is graphene oxide powder.Weigh
Certain powder adds deionized water, ultrasonic vibration, you can obtain graphene oxide dispersion.
Embodiment 3
Raw material is wanted based on microlite ink powder, acetone is chosen and N- methyl-props network alkanone (NMP) is prepared and peeled off graphite powder.Take
20mL acetone, 80mLN- methyl-props network alkanone (NMP).2g microlite ink powders are taken, in adding mixed liquor, ultrasound shake under airtight condition
Swing, keeping temperature is not higher than 50 DEG C, and the concussion time is 6 hours.
After the completion of, filter paper is filtered, then is dried 6 hours at 50 DEG C, obtains desciccate.
Take 1g desciccates, add 0.5g sodium nitrate, the 43g concentrated sulfuric acids are placed in ice bath with magnetic agitation 3 hours,
Keeping temperature is 5 DEG C.
Under condition of ice bath and continue agitating solution, be slowly added to 3g potassium permanganate, it is ensured that add potassium permanganate mistake
Cheng Zhong, solution temperature is not above 10 DEG C.Treat that potassium permanganate starts timing after all adding, stirring reaction is continued under ice bath
2 hours.Beaker is moved in 40 DEG C of tepidariums, stirring reaction 7 hours.Again property adds 3g potassium permanganate, in 40 DEG C of warm water
12 hours are stirred in bath.Product is cooled to after room temperature, is sprinkled on the ice cube containing 20% aqueous hydrogen peroxide solution.Stir
During mixing, then hydrogenperoxide steam generator is added dropwise, obtains graphite oxide.
By being cleaned multiple times, after collecting solid, it is dried 12 hours below 60 DEG C, this is graphene oxide powder.Weigh
Certain powder adds deionized water, ultrasonic vibration, you can obtain graphene oxide dispersion.
Although describing the embodiment for determining, these embodiments only occur as example, and are not intended to limit
The scope of the present invention.In fact, new embodiment described herein can be revised as any other form；Furthermore it is possible to not take off
Under the spirit of the present invention, the pro forma different omission of embodiment described here is carried out, is substituted and is changed, when falling
When entering in scope and spirit of the present invention, accessory claim and its equivalent are intended to cover such form or modification.
Claims (12)
1. a kind of preparation method of graphene oxide, it is characterised in that：The method is comprised the following steps：
(1) graphite suspension is prepared：With common graphite powder as raw material, the stone containing thin graphite flake layer is obtained using liquid phase stripping method
Black suspension；
(2) graphite flake powder is prepared：To graphite suspension obtained in step (1), filtered and be dried, obtained graphite flake
Powder；
(3) intercalation：Solvent is added in graphite flake powder obtained in step (2), intercalation is carried out；
(4) graphite oxide is prepared：To step (3) resulting solution, ice method is sprinkled by oxidation oxidation stone is formed at 20 DEG C -40 DEG C
Ink；
(5) clean and ultrasonically treated：Graphite oxide obtained in step (4) is cleaned and is dried；It is subsequently adding deionized water
Or organic solvent, and carry out ultrasonically treated, obtain the graphene oxide dispersion containing graphene oxide.
2. the preparation method of graphene oxide according to claim 1, it is characterised in that：It is described general in the step (1)
Logical graphite powder is selected from crystalline graphite powder, expansible graphite powder or microcrystal graphite powder.
3. the preparation method of graphene oxide according to claim 1, it is characterised in that：In the step (1), the liquid
Phase stripping method detailed process is：Common graphite powder is added in liquid solution, the weight of the common graphite powder is liquid solution
The 0.1-2% of weight, at 20 DEG C -50 DEG C of temperature and airtight condition, is shaken with the ultrasonic wave more than or equal to 80 watts of power
Swing or grind, concussion or milling time are 1-12 hours.
4. the preparation method of graphene oxide according to claim 3, it is characterised in that：The liquid solution is selected from following
One of mixed liquor：
Deionized water and acetone mixture, wherein acetone are 70-90wt%；Or
Acetone and alcohol mixeding liquid, wherein acetone are 70-90wt%；Or
Acetone and N- methyl-prop network alkanone mixed liquors, wherein acetone are 10-30wt%.
5. the preparation method of graphene oxide according to claim 1, it is characterised in that：The filtration step of the step (2)
In rapid, using ordinary filter paper or membrane filtration, the ordinary filter paper is the qualitative or quantitative filter paper of experiment.
6. the preparation method of graphene oxide according to claim 1, it is characterised in that：Being dried for the step (2) is walked
In rapid, baking temperature is 40 DEG C -90 DEG C, and the time is 6-12 hours.
7. the preparation method of graphene oxide according to claim 1, it is characterised in that：In the step (3), by graphite
Flake powder and solvent mixture are placed in ice bath with magnetic agitation 2-4 hour, and keeping temperature is between 0 DEG C -5 DEG C, to make graphite
Flake powder is sufficiently mixed with solvent.
8. the preparation method of graphene oxide according to claim 1, it is characterised in that：It is described to insert in the step (3)
Layer reaction dissolvent is the combination of sodium nitrate and the concentrated sulfuric acid, or for the combination of red fuming nitric acid (RFNA) and the concentrated sulfuric acid.
9. the preparation method of graphene oxide according to claim 8, it is characterised in that：Graphite flake powder and sodium nitrate
It is 2 with the part by weight of the concentrated sulfuric acid：1：80-100；Graphite flake powder is 1 with the part by weight of red fuming nitric acid (RFNA) and the concentrated sulfuric acid：15-
20：55-70.
10. the preparation method of graphene oxide according to claim 1, it is characterised in that：It is described in the step (4)
Ice method detailed process is sprinkled in oxidation：
Under condition of ice bath, continue whipping step (3) resulting solution, be slowly added to potassium permanganate, the potassium permanganate with it is described
The weight ratio of common graphite powder is 3：1, during potassium permanganate is added, solution temperature is not higher than 10 DEG C；Treat that potassium permanganate is complete
Portion starts timing after adding, and stirring reaction 0.5-2 hour is continued under ice bath；Now, solution is blackish green；Beaker is moved to
In 20 DEG C of -40 DEG C of tepidariums, stirring reaction 6-8 hour；
Then, potassium permanganate is disposably added, the potassium permanganate is 3 with the weight ratio of the common graphite powder：1,20 DEG C-
8-12 hours are stirred in 40 DEG C of tepidariums；Product is cooled to after room temperature, is sprinkled water-soluble containing 5-30% hydrogen peroxide
On the ice cube of liquid, and stir, in whipping process, then hydrogenperoxide steam generator is added dropwise, it is molten that solution can become glassy yellow from reddish brown
Liquid, obtains graphite oxide in ie in solution.
The preparation method of 11. graphene oxides according to claim 1, it is characterised in that：In the step (5), use
Deionized water carries out cleaning operation.
The preparation method of 12. graphene oxides according to claim 1, it is characterised in that：The organic solvent is N- first
Base the third network alkanone NMP, dimethylformamide DMF or dimethyl sulfoxide (DMSO) DMSO.
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| CN107043104A (en) * | 2017-05-11 | 2017-08-15 | 桂林理工大学 | A kind of graphene quantum dot induces high nitrogen doped photo-reduction graphene oxide preparation method |
| CN107697911A (en) * | 2017-10-18 | 2018-02-16 | 复旦大学 | A kind of method that graphite oxide prepares native graphite heat dissipation film |
| CN107720739A (en) * | 2017-09-30 | 2018-02-23 | 湖南国盛石墨科技有限公司 | The preparation method of micro crystal graphite alkene |
| CN107867685A (en) * | 2017-10-18 | 2018-04-03 | 复旦大学 | A kind of preparation method of the native graphite heat dissipation film of high heat conductance |
| CN110265542A (en) * | 2019-07-09 | 2019-09-20 | 山东光韵智能科技有限公司 | A kind of high risk zone radiation protection high energy light absorption transition material and its manufacturing method |
| CN110272039A (en) * | 2018-03-15 | 2019-09-24 | 中国科学院宁波材料技术与工程研究所 | A kind of high-concentration biological base two-dimensional material dispersion liquid, preparation method and application |
| CN110980717A (en) * | 2019-10-29 | 2020-04-10 | 广东墨睿科技有限公司 | Method for preparing graphene oxide by using vermicular graphite |
| CN111704126A (en) * | 2020-05-14 | 2020-09-25 | 上海大学 | Reduction method of graphene oxide |
| CN112408371A (en) * | 2020-10-30 | 2021-02-26 | 宁波石墨烯创新中心有限公司 | Graphene heat-conducting film, preparation method thereof and electronic equipment |
| CN112479196A (en) * | 2020-06-11 | 2021-03-12 | 中科远方(北京)科技有限公司 | Graphene oxide and preparation method thereof |
| CN114203923A (en) * | 2021-12-07 | 2022-03-18 | 深圳市华星光电半导体显示技术有限公司 | Hole buffer material, preparation method thereof and OLED device |
| CN114940492A (en) * | 2022-05-06 | 2022-08-26 | 赵庆华 | Graphene powder deep processing technology by fixed connection liquid dispersion method |
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| CN107697911A (en) * | 2017-10-18 | 2018-02-16 | 复旦大学 | A kind of method that graphite oxide prepares native graphite heat dissipation film |
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| CN112408371A (en) * | 2020-10-30 | 2021-02-26 | 宁波石墨烯创新中心有限公司 | Graphene heat-conducting film, preparation method thereof and electronic equipment |
| CN114203923A (en) * | 2021-12-07 | 2022-03-18 | 深圳市华星光电半导体显示技术有限公司 | Hole buffer material, preparation method thereof and OLED device |
| CN114203923B (en) * | 2021-12-07 | 2023-12-05 | 深圳市华星光电半导体显示技术有限公司 | Hole buffer material, preparation method thereof and OLED device |
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