CN108128769A - A kind of preparation method of the graphene aerogel electrode material of low-cost and high-performance - Google Patents
A kind of preparation method of the graphene aerogel electrode material of low-cost and high-performance Download PDFInfo
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- CN108128769A CN108128769A CN201810112797.2A CN201810112797A CN108128769A CN 108128769 A CN108128769 A CN 108128769A CN 201810112797 A CN201810112797 A CN 201810112797A CN 108128769 A CN108128769 A CN 108128769A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
- H01M4/587—Carbonaceous material, e.g. graphite-intercalation compounds or CFx for inserting or intercalating light metals
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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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
- Y02E60/10—Energy storage using batteries
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Abstract
The invention belongs to nano-functional material preparation method technical fields, and in particular to a kind of preparation method of the graphene aerogel electrode material of low-cost and high-performance.Graphene oxide dispersion is prepared, and the graphene oxide dispersion and amine curing agent are uniformly mixed to get graphene oxide liquid mixture using stripping graphite oxide method；The amine curing agent is diaminodiphenyl-methane, one kind in diaminodiphenylsulfone, diethylenetriamines, trien；Graphene oxide liquid mixture sealing is placed in 90~110 DEG C of environment and is heated, makes amine curing agent redox graphene, obtains graphene hydrogel；By step（2）It is put into vacuum freeze drier after the graphene hydrogel precooling of gained, 45~70h is freezed at -20 DEG C, obtains graphene aerogel electrode material.The preparation method of the present invention is simple and environmentally-friendly, controllable, is easy to industrialized production, and graphene obtained plays gel novel and unique, great novelty.
Description
Technical field
The invention belongs to nano-functional material preparation method technical fields, and in particular to a kind of graphite of low-cost and high-performance
The preparation method of alkene gas gel electrode material.
Background technology
Graphene aerogel electrode material has good elastic characteristic in itself, is very suitable for the electricity as flexible battery
Pole material uses, available for a kind of flexible lithium of electrode material structure of graphene aerogel composite material as lithium ion battery
Ion battery makes full use of bi-dimensional cellular shape structure, very high conductivity and the thermal conductivity of graphene, functionalized surface, simultaneously
Easy processing into fexible film, big specific surface area can load more active materials the features such as on the basis of flexibility is realized into one
Step improves its chemical property.Can be realized when grapheme material is as electrode flexibility can improve again battery integral energy it is close
Degree.
At present, the preparation method of graphene aerogel electrode material is mainly in the majority with self assembly and phase transfer method, hydro-thermal system
Preparation Method is less.Self assembly and phase transfer method preparation process are complicated, and process should not control, and production cost is high, to environment
There is certain pollution.
Invention content
The overcome the deficiencies in the prior art during purpose of the present invention and a kind of graphene aerogel of low-cost and high-performance is provided
The preparation method of electrode material, it is simple and environmentally-friendly, controllable, it is easy to industrialized production, graphene obtained plays gel novel and unique, pole
Tool is innovative.
A kind of preparation method of the graphene aerogel electrode material of low-cost and high-performance has according to following steps reality
It applies：
（1）Graphene oxide dispersion is prepared, and by the graphene oxide dispersion and amine using stripping graphite oxide method
Curing agent is uniformly mixed to get graphene oxide liquid mixture；
Wherein, the amine curing agent is diaminodiphenyl-methane, diaminodiphenylsulfone, diethylenetriamines, Sanya second
One kind in urotropine；
（2）Graphene oxide liquid mixture sealing is placed in 90~110 DEG C of environment and is heated, makes amine curing agent oxygen reduction
Graphite alkene obtains graphene hydrogel；
（3）By step（2）It is put into vacuum freeze drier after the graphene hydrogel precooling of gained, 45 is freezed at -20 DEG C
~70h obtains graphene aerogel electrode material.
Step（1）In, the graphene oxide dispersion specific make step is：Dissolve polyvinyl alcohol in distilled water
Middle ultrasonic disperse is made polyvinyl alcohol water solution, then solid oxidation graphene ultrasonic disperse is obtained in polyvinyl alcohol water solution
The graphene oxide dispersion of a concentration of 2~10mg/ml.
A concentration of 2.5 mg/ml of the polyvinyl alcohol water solution.
Step（1）In, the mass ratio of graphene oxide and amine curing agent is 1 in the graphene oxide liquid mixture：10
~1：100, a concentration of 2~8mg/ml of graphene oxide in gained graphene oxide liquid mixture.
The invention has the advantages that:The preparation method of the present invention is simple and environmentally-friendly, controllable, is easy to industrialized production,
Graphene obtained plays gel novel and unique, great novelty.
Specific embodiment
Embodiment 1
（1）Graphene oxide dispersion is prepared using stripping graphite oxide method, dissolves polyvinyl alcohol in ultrasound point in distilled water
It dissipates obtained 2.5 mg/ml polyvinyl alcohol water solutions, then solid oxidation graphene ultrasonic disperse is obtained in polyvinyl alcohol water solution
The graphene oxide dispersion of a concentration of 2mg/ml；
（2）Prepare graphene oxide liquid mixture：Diaminodiphenyl-methane is evenly spread in graphene oxide dispersion, is obtained
To graphene oxide liquid mixture, the wherein mass ratio of graphene oxide and diaminodiphenyl-methane is 1：10, gained oxidation stone
A concentration of 2mg/ml of graphene oxide in black alkene mixed liquor.
（3）Graphene oxide liquid mixture sealing is placed in 90 DEG C of environment and is heated, makes diaminodiphenyl-methane
Redox graphene obtains graphene hydrogel；
（4）By step（3）It is put into vacuum freeze drier after the graphene hydrogel precooling of gained, is freezed at -20 DEG C
45h obtains graphene aerogel electrode material.
Embodiment 2
（1）Graphene oxide dispersion is prepared using stripping graphite oxide method, dissolves polyvinyl alcohol in ultrasound point in distilled water
It dissipates obtained 2.5 mg/ml polyvinyl alcohol water solutions, then solid oxidation graphene ultrasonic disperse is obtained in polyvinyl alcohol water solution
The graphene oxide dispersion of a concentration of 10mg/ml；
（2）Prepare graphene oxide liquid mixture：Diaminodiphenylsulfone is evenly spread in graphene oxide dispersion, obtains oxygen
Graphite alkene mixed liquor, the wherein mass ratio of graphene oxide and diaminodiphenyl-methane are 1：100, gained graphene oxide
A concentration of 8mg/ml of graphene oxide in mixed liquor.
（3）Graphene oxide liquid mixture sealing is placed in 110 DEG C of environment and is heated, restores diaminodiphenylsulfone
Graphene oxide obtains graphene hydrogel；
（4）By step（3）It is put into vacuum freeze drier after the graphene hydrogel precooling of gained, is freezed at -20 DEG C
70h obtains graphene aerogel electrode material.
Embodiment 3
（1）Graphene oxide dispersion is prepared using stripping graphite oxide method, dissolves polyvinyl alcohol in ultrasound point in distilled water
It dissipates obtained 2.5 mg/ml polyvinyl alcohol water solutions, then solid oxidation graphene ultrasonic disperse is obtained in polyvinyl alcohol water solution
The graphene oxide dispersion of a concentration of 4mg/ml；
（2）Prepare graphene oxide liquid mixture：Diaminodiphenyl-methane is evenly spread in graphene oxide dispersion, is obtained
To graphene oxide liquid mixture, the wherein mass ratio of graphene oxide and diaminodiphenyl-methane is 1：60, gained oxidation stone
A concentration of 4mg/ml of graphene oxide in black alkene mixed liquor.
（3）Graphene oxide liquid mixture sealing is placed in 100 DEG C of environment and is heated, makes diaminodiphenyl-methane
Redox graphene obtains graphene hydrogel；
（4）By step（3）It is put into vacuum freeze drier after the graphene hydrogel precooling of gained, is freezed at -20 DEG C
50h obtains graphene aerogel electrode material.
Embodiment 4
（1）Graphene oxide dispersion is prepared using stripping graphite oxide method, dissolves polyvinyl alcohol in ultrasound point in distilled water
It dissipates obtained 2.5 mg/ml polyvinyl alcohol water solutions, then solid oxidation graphene ultrasonic disperse is obtained in polyvinyl alcohol water solution
The graphene oxide dispersion of a concentration of 8mg/ml；
（2）Prepare graphene oxide liquid mixture：Diaminodiphenylsulfone is evenly spread in graphene oxide dispersion, obtains oxygen
Graphite alkene mixed liquor, the wherein mass ratio of graphene oxide and diaminodiphenyl-methane are 1：80, gained graphene oxide
A concentration of 6mg/ml of graphene oxide in mixed liquor.
（3）Graphene oxide liquid mixture sealing is placed in 100 DEG C of environment and is heated, restores diaminodiphenylsulfone
Graphene oxide obtains graphene hydrogel；
（4）By step（3）It is put into vacuum freeze drier after the graphene hydrogel precooling of gained, is freezed at -20 DEG C
60h obtains graphene aerogel electrode material.
Claims (4)
1. a kind of preparation method of the graphene aerogel electrode material of low-cost and high-performance, which is characterized in that have according to
Lower step is implemented：
(1) graphene oxide dispersion is prepared using stripping graphite oxide method, and by the graphene oxide dispersion and amine
Curing agent is uniformly mixed to get graphene oxide liquid mixture；
Wherein, the amine curing agent is diaminodiphenyl-methane, diaminodiphenylsulfone, diethylenetriamines, Sanya second
One kind in urotropine；
(2) graphene oxide liquid mixture sealing is placed in 90~110 DEG C of environment and heated, make amine curing agent oxygen reduction
Graphite alkene obtains graphene hydrogel；
(3) it will be put into vacuum freeze drier after the graphene hydrogel precooling obtained by step (2), 45 freezed at -20 DEG C
~70h obtains graphene aerogel electrode material.
2. the preparation method of the graphene aerogel electrode material of low-cost and high-performance according to claim 1, feature
It is, in step (1), the graphene oxide dispersion specific make step is：It dissolves polyvinyl alcohol in distilled water
Ultrasonic disperse is made polyvinyl alcohol water solution, then solid oxidation graphene ultrasonic disperse is obtained dense in polyvinyl alcohol water solution
Spend the graphene oxide dispersion for 2~10mg/ml.
3. the preparation method of the graphene aerogel electrode material of low-cost and high-performance according to claim 2, feature
It is, a concentration of 2.5mg/ml of the polyvinyl alcohol water solution.
4. the preparation method of the graphene aerogel electrode material of low-cost and high-performance according to claim 1, feature
It is, in step (1), the mass ratio of graphene oxide and amine curing agent is 1 in the graphene oxide liquid mixture：10~1：
100, a concentration of 2~8mg/ml of graphene oxide in gained graphene oxide liquid mixture.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201810112797.2A CN108128769A (en) | 2018-02-05 | 2018-02-05 | A kind of preparation method of the graphene aerogel electrode material of low-cost and high-performance |
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| CN201810112797.2A CN108128769A (en) | 2018-02-05 | 2018-02-05 | A kind of preparation method of the graphene aerogel electrode material of low-cost and high-performance |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109052374A (en) * | 2018-08-28 | 2018-12-21 | 浙江工业大学 | Method for quickly preparing graphene aerogel through heteropoly acid catalysis |
| CN109437174A (en) * | 2018-11-13 | 2019-03-08 | 江西宏柏新材料股份有限公司 | A kind of doping carbonization C60The preparation method of the graphene aerogel combination electrode material of micro-strip |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103537236A (en) * | 2013-10-22 | 2014-01-29 | 中国科学院宁波材料技术与工程研究所 | Preparation method of graphene aerogel |
| CN104843676A (en) * | 2014-12-03 | 2015-08-19 | 北汽福田汽车股份有限公司 | Preparation method for graphene aerogel |
| CN106082202A (en) * | 2016-06-29 | 2016-11-09 | 北京化工大学 | A kind of preparation method and application of graphene aerogel |
-
2018
- 2018-02-05 CN CN201810112797.2A patent/CN108128769A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103537236A (en) * | 2013-10-22 | 2014-01-29 | 中国科学院宁波材料技术与工程研究所 | Preparation method of graphene aerogel |
| CN104843676A (en) * | 2014-12-03 | 2015-08-19 | 北汽福田汽车股份有限公司 | Preparation method for graphene aerogel |
| CN106082202A (en) * | 2016-06-29 | 2016-11-09 | 北京化工大学 | A kind of preparation method and application of graphene aerogel |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109052374A (en) * | 2018-08-28 | 2018-12-21 | 浙江工业大学 | Method for quickly preparing graphene aerogel through heteropoly acid catalysis |
| CN109052374B (en) * | 2018-08-28 | 2020-05-22 | 浙江工业大学 | Method for quickly preparing graphene aerogel through heteropoly acid catalysis |
| CN109437174A (en) * | 2018-11-13 | 2019-03-08 | 江西宏柏新材料股份有限公司 | A kind of doping carbonization C60The preparation method of the graphene aerogel combination electrode material of micro-strip |
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Application publication date: 20180608 |