CN110156003A - A kind of graphene oxide dispersion and preparation method thereof - Google Patents
A kind of graphene oxide dispersion and preparation method thereof Download PDFInfo
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- CN110156003A CN110156003A CN201910566257.6A CN201910566257A CN110156003A CN 110156003 A CN110156003 A CN 110156003A CN 201910566257 A CN201910566257 A CN 201910566257A CN 110156003 A CN110156003 A CN 110156003A
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- graphene oxide
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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
- C01B32/19—Preparation by exfoliation
- C01B32/192—Preparation by exfoliation starting from graphitic oxides
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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
- C01B32/198—Graphene oxide
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/24—Electrodes characterised by structural features of the materials making up or comprised in the electrodes, e.g. form, surface area or porosity; characterised by the structural features of powders or particles used therefor
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
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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
- C01B2204/00—Structure or properties of graphene
- C01B2204/20—Graphene characterized by its properties
- C01B2204/22—Electronic properties
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/13—Energy storage using capacitors
Abstract
Type of the present invention discloses a kind of graphene oxide dispersion and preparation method thereof, and the graphene oxide light transmission of preparation is good, and comparative surface area is big, as tulle.Also disclose the method for preparation graphene oxide dispersion, comprising: (1) glassy yellow reactant is prepared using the reaction of the chemicals such as graphite powder, the concentrated sulfuric acid, phosphoric acid, potassium permanganate, hydrogen peroxide.(2) dilute hydrochloric acid solution is added and washs mixed reactant, then use deionized water, wash repeatedly, be washed till neutrality, be freeze-dried.(3) finally the graphite oxide powder of certain mass is add to deionized water, ultrasound removing is configured to the graphene oxide dispersion of required concentration.The raw materials used in the present invention is easy to get, and technology maturation, cost is relatively low, short preparation period, operating process is simple and easy to control, and graphene oxide light transmittance obtained is good, comparative surface area is big, is in gauze-like, has higher conductivity, has outstanding cyclical stability as electrode material.
Description
Technical field
The present invention relates to a kind of preparation methods of graphene oxide dispersion.
Background technique
With the progress of the mankind and the fast development of science and technology, the fossil energy that can not be reused on the earth cannot expire
For the sufficient mankind increasingly to the demand of the energy, petroleum resources are increasingly short, and the exhaust gases of internal combustion engines of burning petroleum can cause it is a series of
Environmental problem.Therefore energy problem has become one of most pressing problem of facing mankind, has influenced people
Daily life and the environment that we depend on for existence.Therefore, people are such as new in the high efficient energy sources device of research substitution internal combustion engine
Type energy storage device, clean reproducible energy etc. cater to demand of the human future to the energy with this.In recent years, people
Sight is focused on the research and development of high efficient energy sources storage device above, wherein indispensable a part is stored to electrochemical energy
The research of device, probing on solar battery, lithium ion battery, fuel cell achieve very big achievement, but not
Have and solves their intrinsic fatal defects.As the lower power density of lithium ion battery, the higher cost of manufacture of solar battery,
Biggish security risk of fuel cell etc., in application aspect, there is also -- fixed bottlenecks.Supercapacitor is met the tendency of in this context
And give birth to, because it is with some unique characteristics, including higher power density, excellent cyclical stability, the charge and discharge being exceedingly fast
Rate and cost of manufacture are lower etc..However the energy density of supercapacitor is well below lithium ion battery, in some aspects
Limit its large-scale application.Therefore, how while guaranteeing its higher power density its energy density and invertibity to be improved
It is the direction that scientific research is made great efforts.Researchers mainly improved supercapacitor by following several respects in recent years
Relevant nature: (1) electrode material electric conductivity is improved；(2) it makes porous material and guarantees appropriate pore size distribution range；(3)
Improve the wellability of electrode material；(4) bulk density of material is improved；So researchers have been carried out to metal oxygen
Compound, the research of carbon material and some other composite material achieve certain effect.It is excellent that water soluble characteristic is prepared in the present invention
Different graphene oxide dispersion, for graphene and other materials it is compound after in supercapacitor using provide one kind can
Energy.
Summary of the invention
The technical problems to be solved by the present invention are: with the change such as graphite powder, the concentrated sulfuric acid, phosphoric acid, potassium permanganate, hydrogen peroxide
Drug is raw material, carries out preparing graphite oxide by the method for chemical reaction.The raw materials used in the present invention is easy to get, technology maturation,
Cost is relatively low, short preparation period, safe operation process, simple, easily-controllable, graphene oxide good water solubility obtained, and light transmittance is high,
Comparative surface area is big, it is fluffy, be in gauze-like, have higher conductivity, there is outstanding stable circulation as electrode composite material
Property.
The present invention provides the preparation methods of graphene oxide dispersion, comprising the following steps: step S1: with graphite powder,
Glassy yellow reactant is prepared in the reaction of the chemicals such as the concentrated sulfuric acid, phosphoric acid, potassium permanganate, hydrogen peroxide；Step S2: reactant
It is washed till neutrality, is freeze-dried；Step S3: the graphite oxide powder of certain mass is added in deionized water, and ultrasound removing is prepared
At the graphene oxide dispersion of required concentration.
Further, the preparation method of the graphene oxide dispersion, it is characterised in that: in the step S1, first
By 2.0g graphite powder be added on equipped with the 360.0mL concentrated sulfuric acid, 40.0mL phosphoric acid round-bottomed flask in, be sufficiently stirred 30 minutes
Afterwards, it is slowly added to 18.0g potassium permanganate, then improves temperature to 50 degrees Celsius of sustained response 16h.After the reaction was completed, zero
In the system of degree, 400.0mL deionized water is added in reactor, movement slowly will avoid temperature from increasing too fast.Then will
The hydrogenperoxide steam generator of 20.0mL or so is slowly added in mixed liquor, is persistently stirred 30 minutes, the color of solution becomes bright orange
Color.
Further, the preparation method of graphene oxide dispersion, it is characterised in that:, will be in step S1 in the step S2
Obtained reaction product stands a period of time, and upper layer acid waste liquid is poured out, and dilute hydrochloric acid solution (10%) is added later and continues to settle
Upper layer waste liquid is outwelled and dilute hydrochloric acid is added repeatedly, the sulfate radical in solution is ensured after pickling for several times by separation after solution layering
Ion has been completely removed;Then deionized water is added in beaker to be washed repeatedly, until it is washed till neutrality, obtained oxidation
Graphite is tacky, brown colloidal, finally comes out product by centrifuge separation, is put into vacuum freeze drier and gets rid of production
Moisture in object obtains graphite oxide powder.
Further, the preparation method of graphene oxide dispersion, it is characterised in that: in the step S3, by certain mass
Graphite oxide powder be add to deionized water, be configured to required concentration.It is sufficiently stirred after twenty minutes with magnetic stirring apparatus,
It is put into ultrasonic wave and is dispersed, control ultrasonic power, ultrasonic time are obtained with peeling away oxidized graphite flake layer in solution
The graphene oxide dispersion of state.
After above-mentioned technical proposal, the invention has the following advantages: 1) graphene oxide prepared by the present invention
Good dispersion property in aqueous solution has biggish specific surface area, there is higher light transmittance and conductivity, is well suited as super
The electrode material of capacitor；2) present invention preparation graphene oxide dispersion, raw material are easy to get, and cost is relatively low, experimentation
It is safe, simple.
Detailed description of the invention
Fig. 1 is the electron scanning micrograph of graphite oxide of the present invention；Fig. 2 is the transmission electron microscope of graphite oxide of the present invention
Photo；Fig. 3 is that the XRD of graphite oxide powder of the invention schemes.
Specific embodiment
In order that the present invention can be more clearly and readily understood, right below according to specific embodiment and in conjunction with attached drawing
The present invention is described in further detail.
Embodiment one: a kind of graphite oxide observes its pattern by scanning electron microscope and transmission electron microscope.From Fig. 1 oxygen
The electron scanning micrograph of graphite can be seen, the shape characteristic of GO: it is transparent, as tulle.The transmitance of light is good,
This illustrates that GO is very thin in thickness orientation, has reached the standard of graphene, and have very big specific surface area；From Fig. 2 high
This it appears that the texture structure of GO thin layer on times resolution ratio TEM picture, it is considered that single texture is an atomic layers thick
Degree, therefore it is considered that the prepared sample number of plies is average at 3-4 layers, mutually winding superposition causes between graphene oxide layer
Its numerous texture, or due to thermodynamic one, crimp can occur for edge.Meanwhile TEM photo shows graphene oxide
It rises and falls with fold, shaggy shape characteristic；Fig. 3 gives the XRD diagram of graphite oxide, and XRD can analyze out material
Some physical property characteristics, such as the orientation and internal crystallization state of the object phase composition of substance, crystal crystal face in material internal, figure
Nearby there is a stronger characteristic peak in only one diffraction maximum of middle GO, 2 11 ° of the angles θ, and d value is about 7.5, this shows object in sample
Mutually single, the crystallization degree of GO is obvious, positioned at 22 ° of diffraction maximums be graphite characteristic peak, but be located at 11 ° near GO feature
Peak is compared, and is disappeared substantially, from XRD diagram as can be seen that GO has very big interlamellar spacing, demonstrates graphite at through oxidation
The macroscopic appearance that volume obviously expands after reason.
Embodiment two: the present invention provides the preparation methods of graphene oxide dispersion, comprising the following steps: step S1:
Glassy yellow reactant is prepared with the reaction of the chemicals such as graphite powder, the concentrated sulfuric acid, phosphoric acid, potassium permanganate, hydrogen peroxide；Step
S2: reactant is washed till neutrality, freeze-drying；Step S3: the graphite oxide powder of certain mass is added in deionized water, ultrasound
Removing is configured to the graphene oxide dispersion of required concentration.
Preferably, the preparation method of the graphene oxide dispersion, it is characterised in that: in the step S1, first
By 2.0g graphite powder be added on equipped with the 360.0mL concentrated sulfuric acid, 40.0mL phosphoric acid round-bottomed flask in, be sufficiently stirred 30 minutes
Afterwards, it is slowly added to 18.0g potassium permanganate, then improves temperature to 50 degrees Celsius of sustained response 16h.After the reaction was completed, zero
In the system of degree, 400.0mL deionized water is added in reactor, movement slowly will avoid temperature from increasing too fast.Then will
The hydrogenperoxide steam generator of 20.0mL or so is slowly added in mixed liquor, is persistently stirred 30 minutes, the color of solution becomes bright orange
Color.
Preferably, the preparation method of graphene oxide dispersion, it is characterised in that:, will be in step S1 in the step S2
Obtained reaction product stands a period of time, and upper layer acid waste liquid is poured out, and dilute hydrochloric acid solution (10%) is added later and continues to settle
Upper layer waste liquid is outwelled and dilute hydrochloric acid is added repeatedly, the sulfate radical in solution is ensured after pickling for several times by separation after solution layering
Ion has been completely removed;Then deionized water is added in beaker to be washed repeatedly, until it is washed till neutrality, obtained oxidation
Graphite is tacky, brown colloidal, finally comes out product by centrifuge separation, is put into vacuum freeze drier and gets rid of production
Moisture in object obtains graphite oxide powder.
Preferably, the preparation method of graphene oxide dispersion, it is characterised in that: in the step S3, by certain mass
Graphite oxide powder be add to deionized water, be configured to required concentration.It is sufficiently stirred after twenty minutes with magnetic stirring apparatus,
It is put into ultrasonic wave and is dispersed, control ultrasonic power, ultrasonic time are obtained with peeling away oxidized graphite flake layer in solution
The graphene oxide dispersion of state.
The present invention passes through chemistry using chemicals such as graphite powder, the concentrated sulfuric acid, phosphoric acid, potassium permanganate, hydrogen peroxide as raw material
Prepared by the method for reaction, the raw materials used in the present invention is easy to get, and technology maturation, cost is relatively low, short preparation period, operating process letter
Single easily-controllable, graphene oxide good water solubility obtained, light transmittance is high, comparative surface area is big, it is fluffy, be in gauze-like, have higher
Conductivity has outstanding cyclical stability as electrode material.
Particular embodiments described above, pair present invention solves the technical problem that, technical scheme and beneficial effects carry out
It is further described, it should be understood that the above is only a specific embodiment of the present invention, is not limited to this
Invention, all within the spirits and principles of the present invention, any modification, equivalent substitution, improvement and etc. done should be included in this hair
Within bright protection scope.
Claims (5)
1. a kind of graphene oxide, it is characterised in that: with chemistry such as graphite powder, the concentrated sulfuric acid, phosphoric acid, potassium permanganate, hydrogen peroxide
Drug is raw material, is prepared by the method for chemical reaction, and the raw materials used in the present invention is easy to get, and technology maturation, cost is relatively low, system
The standby period is short, and operating process is simple and easy to control, graphene oxide good water solubility obtained, and light transmittance is high, and comparative surface area is big, is in thin
Yarn shape has higher conductivity, has outstanding cyclical stability as electrode material.
2. the preparation method of graphene oxide dispersion according to claim 1, comprising the following steps: step S1: use stone
Glassy yellow reactant is prepared in the reaction of the chemicals such as ink powder, the concentrated sulfuric acid, phosphoric acid, potassium permanganate, hydrogen peroxide；Step S2:
Reactant is washed till neutrality, is freeze-dried；Step S3: the graphite oxide powder of certain mass is added in deionized water, ultrasound
Removing is configured to the graphene oxide dispersion of required concentration.
3. the preparation method of graphene oxide dispersion according to claim 2, it is characterised in that: in the step S1,
First by 2.0g graphite powder be added on equipped with the 360mL concentrated sulfuric acid, 40mL phosphoric acid round-bottomed flask in, be sufficiently stirred 30 minutes
Afterwards, it is slowly added to 18g potassium permanganate, then improves temperature to 50 degrees Celsius of sustained response 16h, after the reaction was completed, in zero degree
System in, 400mL deionized water is added in reactor, movement will slowly, avoid temperature increase it is too fast, then by 20mL a left side
Right hydrogenperoxide steam generator is slowly added in mixed liquor, is persistently stirred 30 minutes, the color of solution becomes glassy yellow.
4. the preparation method of graphene oxide dispersion according to claim 2, it is characterised in that: in the step S2,
Reaction product obtained in step S1 is stood into a period of time, upper layer acid waste liquid is poured out, dilute hydrochloric acid solution is added later
(10%) continue sedimentation separation to outwell upper layer waste liquid after solution layering and dilute hydrochloric acid is added repeatedly, ensure after pickling for several times
Sulfate ion in solution has been completely removed；Then deionized water is added in beaker to be washed repeatedly, until being washed till
Neutrality, obtained graphite oxide is tacky, brown colloidal, finally comes out product by centrifuge separation, is put into vacuum refrigeration
The moisture in product is got rid of in drying machine, obtains graphite oxide powder.
5. the preparation method of graphene oxide dispersion according to claim 2, it is characterised in that: in the step S3,
The graphite oxide powder of certain mass is add to deionized water, required concentration is configured to, is sufficiently stirred with magnetic stirring apparatus
It mixes after twenty minutes, is put into ultrasonic wave and is dispersed, control ultrasonic power, ultrasonic time peel away oxidized graphite flake layer,
Obtain the graphene oxide dispersion in solution state.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112940835A (en) * | 2021-02-27 | 2021-06-11 | 郝宝民 | Graphene lubricating oil and preparation method thereof |
| CN113194556A (en) * | 2021-04-20 | 2021-07-30 | 广东温道百镒健康科技有限公司 | Graphene radiation heating film and preparation method thereof |
| CN114015323A (en) * | 2021-11-25 | 2022-02-08 | 姚焕芹 | Preparation method of anticorrosive wear-resistant paint |
| CN114975949A (en) * | 2022-06-13 | 2022-08-30 | 鸡西市唯大新材料科技有限公司 | Preparation method of lithium ion carbon negative electrode material |
-
2019
- 2019-06-27 CN CN201910566257.6A patent/CN110156003A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112940835A (en) * | 2021-02-27 | 2021-06-11 | 郝宝民 | Graphene lubricating oil and preparation method thereof |
| CN113194556A (en) * | 2021-04-20 | 2021-07-30 | 广东温道百镒健康科技有限公司 | Graphene radiation heating film and preparation method thereof |
| CN114015323A (en) * | 2021-11-25 | 2022-02-08 | 姚焕芹 | Preparation method of anticorrosive wear-resistant paint |
| CN114975949A (en) * | 2022-06-13 | 2022-08-30 | 鸡西市唯大新材料科技有限公司 | Preparation method of lithium ion carbon negative electrode material |
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