CN110155995A - A kind of High-performance graphene preparation method for lithium ion battery - Google Patents
A kind of High-performance graphene preparation method for lithium ion battery Download PDFInfo
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- CN110155995A CN110155995A CN201810114087.3A CN201810114087A CN110155995A CN 110155995 A CN110155995 A CN 110155995A CN 201810114087 A CN201810114087 A CN 201810114087A CN 110155995 A CN110155995 A CN 110155995A
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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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- 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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- 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
Abstract
The invention discloses a kind of High-performance graphene preparation methods for lithium ion battery, include the following steps: A) carbon source and metal agent for capturing are mixed, modified carbon source is obtained, the carbon source includes one or more of ion exchange resin, starch, cellulose and amorphous carbon；B) by metallic catalyst and the step A) in modification carbon source mix, adsorbed, obtain the modification carbon source for being adsorbed with metallic catalyst；(C) graphite and surfactant are mixed, obtains modified graphite；(D) polymer is mixed with the modified graphite in the step (C), is adsorbed, obtains the modified graphite for being adsorbed with polymer；(E) chain extender is carried out heating with the modification carbon source for being adsorbed with metallic catalyst with the modified graphite for being adsorbed with polymer in the step (D) to mix, finally shearing removing obtains graphene in shearing equipment.Preparation method provided by the invention is at low cost, easy to operate, it is easy to accomplish the industrialized production of graphene.
Description
Technical field
The present invention relates to a kind of preparation method, specifically a kind of High-performance graphene preparation side for lithium ion battery
Method.
Background technique
Lithium ion battery is a kind of secondary rechargeable battery, relies primarily on lithium ion mobile working between a positive electrode and a negative electrode,
In charge and discharge process, lithium ion insertion and deintercalation back and forth between positive and negative two electrodes.Lithium battery interior uses helically coiling
Or stack structure structure, it is made of anode, diaphragm, cathode, organic electrolyte, battery case.Filled with organic polymer electricity in battery
Electrolyte solution.Constitute entire polymer lithium electricity charge and discharge cycles system.Positive electrode occupies larger proportion in lithium ion battery, just
The mass ratio of negative electrode material is 3:1~4:1.Anode material for lithium-ion batteries occupies core status, lithium-ion electric in lithium battery
The performance of pond positive electrode directly affects the performance indexes of lithium ion battery, the cost of the positive electrode of lithium battery
Directly determine battery cost height.The positive electrode of commercial lithium example battery is mostly LiFePO4, LiMn2O4, cobalt acid at present
A small amount of LiMn2O4 is added in lithium, nickle cobalt lithium manganate and nickle cobalt lithium manganate (ternary material).Those material energy densities height, price
It is cheap, safety is excellent, the development especially suitable for power battery.But the resistivity of these positive electrodes is big, electrode material
Utilization rate is low.And the positive electrode of business lithium battery is attached in collector plate, in order to increase between positive electrode and collector plate
Electric conductivity and adhesive force, increased conductive agent and binder, reduce the storage of lithium battery between positive electrode and collector plate
Can density, generate larger resistance and thermal resistance, in battery use process, lithium ion battery made to generate heat, cause service life of lithium battery it is short,
Multiplying power is low, Nei Regao, utilization rate are low.Graphene is the only one layer of original for being stripped out from graphite material, being made of carbon atom
The two dimensional crystal of sub- thickness.Graphene is as new material, specific surface and superpower electric conductivity with superelevation.High-ratio surface is special
Property leads to graphene, and with big DBP value, imbibition and liquid-keeping property are that general conductive agent is incomparable.It is electric under graphene room temperature
Transport factor is more than 15000cm2/Vs, and higher than carbon nanotubes or silicon crystal, electronics has reached the light velocity in movement velocity wherein
1/300, considerably beyond movement velocity of the electronics in general conductor.And the resistivity of graphene is only about 1 Ω m, than
Copper or silver are lower, for the material that resistivity in the world is minimum, electric conductivity is best.Using graphene leading as commercial Li-ion batteries
Electric agent can greatly enhance the conductive capability of lithium ion battery, but the cost of grapheme material is high, leads to lithium ion battery
Cost is too high, is unfavorable for promoting and applying.
Summary of the invention
The purpose of the present invention is to provide a kind of High-performance graphene preparation methods for lithium ion battery, on solving
State the problem of proposing in background technique.
To achieve the above object, the invention provides the following technical scheme:
A kind of High-performance graphene preparation method for lithium ion battery, includes the following steps: A) carbon source and metal are captured
Agent mixing, obtains modified carbon source, the carbon source include one of ion exchange resin, starch, cellulose and amorphous carbon or
It is several；B) by metallic catalyst and the step A) in modification carbon source mix, adsorbed, obtain being adsorbed with metallic catalyst
Modification carbon source；(C) graphite and surfactant are mixed, obtains modified graphite；It (D) will be in polymer and the step (C)
Modified graphite mixing, adsorbed, obtain the modified graphite for being adsorbed with polymer；It (E) will be in chain extender and the step (D)
The modified graphite for being adsorbed with polymer carry out heating with the modification carbon source for being adsorbed with metallic catalyst and mix, finally set in shearing
Standby middle shearing removing obtains graphene.
As a further solution of the present invention: the graphite in the step (C) is crystalline flake graphite, expanded graphite, thermal cracking
One of graphite, highly oriented graphite, graphite oxide.
As a further solution of the present invention: the graphite in the step (C) is crystalline flake graphite, expanded graphite, thermal cracking
One of graphite, highly oriented graphite, graphite oxide.
As a further solution of the present invention: the carbon source in the step A includes phenolic resin, styrene resin, ring
One of oxygen resin, charcoal powder, active carbon, mesoporous carbon, starch and cellulose.
Metal agent for capturing in as a further solution of the present invention: the step A) includes organic sulfur heavy metal chelating
Agent, phosphoric acid salt metal agent for capturing, amino carboxylic acid metalloid agent for capturing, organic phospho acid metalloid agent for capturing and hydroxycarboxylic acid eka-gold
Belong to one of agent for capturing.
As a further solution of the present invention: the phosphoric acid salt metal agent for capturing includes sodium tripolyphosphate, polyphosphoric acids
One or more of sodium, calgon and sodium pyrophosphate；The amino carboxylic acid metalloid agent for capturing includes ethylenediamine tetrem
Acid, aminotriacetic acid, diethylene-triamine pentaacetic acid, N- ethoxy ethamine triacetic acid, ethylene glycol-is bis--(B- amino ethyl ether)-N and
One or more of N- tetraacethyl；The organic phospho acid metalloid agent for capturing include Etidronic Acid, aminotrimethylenephosphonic acid,
In 1- hydroxyl ethylidene -1,1- di 2 ethylhexyl phosphonic acid, ethylene diamine tetra methylene phosphonic acid, diethylene triamine pentamethylene phosphonic and aminotrimethylenephosphonic acid
It is one or more of；The hydroxycarboxylic acid metalloid agent for capturing include sodium nitrilo triacetate, citric acid, tartaric acid, sodium gluconate,
One or more of hydroximic acid, polyacrylic acid and maleic acid.
As further scheme of the invention: the mass ratio of surfactant and the graphite is 1:(10-80).
Compared with prior art, the beneficial effects of the present invention are: preparation method provided by the invention do not use strong acid or
Highly basic is aoxidized, but is catalyzed to obtain graphene, no pollution to the environment using metallic catalyst.Also, it is provided by the invention
Preparation method is modified with metal agent for capturing by carbon source, so that by chelation between metallic catalyst and macromolecule carbon source, it is real
Existing uniform adsorption of the catalyst in the carbon source is handed over so that available carbon source be made to extend further to the small ion of exchange capacity
It changes resin and is not susceptible to the macromolecule carbons such as cellulose of ionic adsorption or ion exchange source；Metal agent for capturing can realize that metal is urged
Uniform adsorption of the agent in carbon source, carbon atom are reset in catalyst surface, graphene thin layer are formed, to obtain quality
It is higher that there is certain three-dimensional structure graphene product.In addition, preparation method provided by the invention is at low cost, it is easy to operate,
It is easily achieved the industrialized production of graphene.
Specific embodiment
The following is a clear and complete description of the technical scheme in the embodiments of the invention, it is clear that described embodiment
Only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, the common skill in this field
Art personnel every other embodiment obtained without making creative work belongs to the model that the present invention protects
It encloses.
In the embodiment of the present invention, a kind of High-performance graphene preparation method for lithium ion battery includes the following steps:
A) carbon source and metal agent for capturing are mixed, obtain modified carbon source, the carbon source include ion exchange resin, starch, cellulose and
One or more of amorphous carbon；B) by metallic catalyst and the step A) in modification carbon source mix, adsorbed, obtained
To the modification carbon source for being adsorbed with metallic catalyst；(C) graphite and surfactant are mixed, obtains modified graphite；It (D) will polymerization
Object is mixed with the modified graphite in the step (C), is adsorbed, and the modified graphite for being adsorbed with polymer is obtained；(E) by chain extension
Agent is heated with the modified graphite for being adsorbed with polymer in the step (D) with the modification carbon source for being adsorbed with metallic catalyst
Mixing, finally shearing removing obtains graphene in shearing equipment.
Graphite in the step (C) is crystalline flake graphite, expanded graphite, thermal cracking graphite, highly oriented graphite, graphite oxide
One of.
Graphite in the step (C) is crystalline flake graphite, expanded graphite, thermal cracking graphite, highly oriented graphite, graphite oxide
One of.
Carbon source in the step A includes phenolic resin, styrene resin, epoxy resin, charcoal powder, active carbon, Jie
One of hole carbon, starch and cellulose.
The step A) in metal agent for capturing include organic sulfur heavy metal chelating agent, phosphoric acid salt metal agent for capturing, ammonia
One of yl carboxylic acid metalloid agent for capturing, organic phospho acid metalloid agent for capturing and hydroxycarboxylic acid metalloid agent for capturing.
The phosphoric acid salt metal agent for capturing includes sodium tripolyphosphate, sodium polyphosphate, calgon and sodium pyrophosphate
One or more of；The amino carboxylic acid metalloid agent for capturing includes ethylenediamine tetra-acetic acid, aminotriacetic acid, diethylentriamine
Pentaacetic acid, N- ethoxy ethamine triacetic acid, ethylene glycol-is bis--(B- amino ethyl ether) one or more of-N and N- tetraacethyl；Institute
Stating organic phospho acid metalloid agent for capturing includes Etidronic Acid, aminotrimethylenephosphonic acid, 1- hydroxyl ethylidene -1,1- di 2 ethylhexyl phosphonic acid, second two
One or more of four methylenephosphonic acid of amine, diethylene triamine pentamethylene phosphonic and aminotrimethylenephosphonic acid；The hydroxycarboxylic acid
Metalloid agent for capturing includes sodium nitrilo triacetate, citric acid, tartaric acid, sodium gluconate, hydroximic acid, polyacrylic acid and maleic acid
One or more of.
The mass ratio of surfactant and the graphite is 1:(10-80).
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 where 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
Benefit requires rather than above description limits, it is intended that all by what is fallen within the meaning and scope of the equivalent elements 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 embodiments being understood that.
Claims (7)
1. a kind of High-performance graphene preparation method for lithium ion battery, which comprises the steps of: A) by carbon
Source and the mixing of metal agent for capturing, obtain modified carbon source, and the carbon source includes ion exchange resin, starch, cellulose and amorphous
One or more of carbon；B) by metallic catalyst and the step A) in modification carbon source mix, adsorbed, adsorbed
There is the modification carbon source of metallic catalyst；(C) graphite and surfactant are mixed, obtains modified graphite；(D) by polymer and institute
The modified graphite mixing in step (C) is stated, is adsorbed, obtains the modified graphite for being adsorbed with polymer；(E) by chain extender and institute
It states the modified graphite for being adsorbed with polymer in step (D) and carries out heating with the modification carbon source for being adsorbed with metallic catalyst and mix,
Finally shearing removing obtains graphene in shearing equipment.
2. the High-performance graphene preparation method according to claim 1 for lithium ion battery, which is characterized in that described
Graphite in step (C) is one of crystalline flake graphite, expanded graphite, thermal cracking graphite, highly oriented graphite, graphite oxide.
3. the High-performance graphene preparation method according to claim 1 for lithium ion battery, which is characterized in that described
Surfactant in step (C) includes octyl phenol polyoxyethylene ether, nonylphenol polyoxyethylene ether, sorbitan ester, fat
One of sour polyoxyethylene ester.
4. the High-performance graphene preparation method according to claim 1 for lithium ion battery, which is characterized in that described
Carbon source in step A includes phenolic resin, styrene resin, epoxy resin, charcoal powder, active carbon, mesoporous carbon, starch and fibre
Tie up one of element.
5. the High-performance graphene preparation method according to claim 1 for lithium ion battery, which is characterized in that described
Step A) in metal agent for capturing include organic sulfur heavy metal chelating agent, phosphoric acid salt metal agent for capturing, amino carboxylic acid metalloid
One of agent for capturing, organic phospho acid metalloid agent for capturing and hydroxycarboxylic acid metalloid agent for capturing.
6. the High-performance graphene preparation method according to claim 5 for lithium ion battery, which is characterized in that described
Phosphoric acid salt metal agent for capturing includes one of sodium tripolyphosphate, sodium polyphosphate, calgon and sodium pyrophosphate or several
Kind；The amino carboxylic acid metalloid agent for capturing includes ethylenediamine tetra-acetic acid, aminotriacetic acid, diethylene-triamine pentaacetic acid, N- hydroxyl
Ethyl ethamine triacetic acid, ethylene glycol-is bis--(B- amino ethyl ether) one or more of-N and N- tetraacethyl；The organic phospho acid
Metalloid agent for capturing includes Etidronic Acid, aminotrimethylenephosphonic acid, 1- hydroxyl ethylidene -1,1- di 2 ethylhexyl phosphonic acid, ethylenediamine tetraacetic methene phosphine
One or more of acid, diethylene triamine pentamethylene phosphonic and aminotrimethylenephosphonic acid；The hydroxycarboxylic acid metalloid captures
Agent include one of sodium nitrilo triacetate, citric acid, tartaric acid, sodium gluconate, hydroximic acid, polyacrylic acid and maleic acid or
It is several.
7. the High-performance graphene preparation method according to claim 1 for lithium ion battery, which is characterized in that surface
The mass ratio of activating agent and the graphite is 1:(10-80).
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| CN104445177A (en) * | 2014-12-16 | 2015-03-25 | 中国科学院宁波材料技术与工程研究所 | Preparation method of graphene, and graphene |
| CN104528696A (en) * | 2014-12-16 | 2015-04-22 | 中国科学院宁波材料技术与工程研究所 | Preparation method for graphene and graphene |
| CN106276881A (en) * | 2016-08-23 | 2017-01-04 | 黄云鸿 | The preparation method of a kind of Graphene and Graphene |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20140263166A1 (en) * | 2009-08-05 | 2014-09-18 | Samsung Electronics Co., Ltd. | Graphene base and method of preparing the same |
| CN104445177A (en) * | 2014-12-16 | 2015-03-25 | 中国科学院宁波材料技术与工程研究所 | Preparation method of graphene, and graphene |
| CN104528696A (en) * | 2014-12-16 | 2015-04-22 | 中国科学院宁波材料技术与工程研究所 | Preparation method for graphene and graphene |
| CN106276881A (en) * | 2016-08-23 | 2017-01-04 | 黄云鸿 | The preparation method of a kind of Graphene and Graphene |
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Application publication date: 20190823 |
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