CN109065219A - A kind of efficient, high dispersive graphene conductive slurry preparation method - Google Patents
A kind of efficient, high dispersive graphene conductive slurry preparation method Download PDFInfo
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- CN109065219A CN109065219A CN201810921764.2A CN201810921764A CN109065219A CN 109065219 A CN109065219 A CN 109065219A CN 201810921764 A CN201810921764 A CN 201810921764A CN 109065219 A CN109065219 A CN 109065219A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/20—Conductive material dispersed in non-conductive organic material
- H01B1/24—Conductive material dispersed in non-conductive organic material the conductive material comprising carbon-silicon compounds, carbon or silicon
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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
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
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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 present invention relates to a kind of efficient, high dispersive graphene conductive slurry preparation methods, --- high speed and high pressure grinding --- three steps of ultrasonic emulsification are mixed by material to constitute, specific step is as follows: (1) by raw graphite, solvent and dispersing agent are by formula rate addition batching kettle, it is stirred evenly under certain temperature, graphite mixed liquor is made；(2) above-mentioned graphite mixed liquor is delivered to high speed grinding unit, material enters pans after high speed grinding, then is transported in high pressure abrasive machine and handles；(3) material after high pressure abrasive is delivered to ultrasonic sound appratus group by pump, the material after ultrasound removing enters emulsifier unit and carries out emulsification treatment, keeps graphene distribution more uniform, obtain graphene conductive slurry finished product after emulsification, is delivered to finished pot storage.The present invention has the advantages that the graphene quality with higher that the present invention obtains, electrocondution slurry dispersibility with higher give full play to its excellent electric conductivity；And have the advantages that the service life is long, weight is low etc..
Description
Technical field
The invention belongs to conductive agent technical field, in particular to a kind of efficient, high dispersive graphene conductive slurry preparation
Method.
Background technique
Currently, the method for preparing graphene mainly has physical method and chemical method.Physical method is mainly the object by storeroom
The graphene with intrinsic property is prepared in reason effect, and it is more completely chemical structure, material that the graphene of this method preparation, which has,
Material performance will not be destroyed, but graphene unstable quality, including mechanical stripping method, arc discharge method, ultrasonic method obtained etc..
Mainly pass through chemical reaction prepares graphene to chemical method, and the graphene quality of method preparation is relatively stable, but chemically reacts
The intrinsic structure of graphene may be destroyed in journey, cause the reduced performance of graphene.Stone is such as prepared using oxidation-reduction method
In black alkene materials process, oxygen-containing group destroys the sp in graphene2Hybridized orbit forms sp3Hybridized orbit greatly drops
The low electric conductivity of graphene.Chemical method mainly has organic synthesis method, chemical vapour deposition technique, oxidation-reduction method etc..It is logical
Prolonged research is crossed, the method for preparing graphene is more and more, and technology is also gradually improved, large-scale production is realized,
But it is rarely reported about application of the graphene in electrocondution slurry.
Conductive agent is usually added into pole piece production a certain amount of to guarantee that electrode has good charge-discharge performance
Conductive materials play the role of collecting micro-current between active material, between active material and collector, to reduce electrode
Contact resistance accelerates the rate travel of electronics, while can also effectively improve migration rate of the lithium ion in electrode material, from
And improve the efficiency for charge-discharge of electrode.
Therefore, conductive agent is increasingly widely used in lithium ion battery.Currently used for lithium ion battery
Conductive agent mainly includes carbon black, graphite, carbon nanotube, carbon nano-fiber and graphene etc..The usage of these conductive agents routine is
It is directly appended to be dispersed in positive and negative pole material, find in actual application, which exists conductive
The uneven problem of agent dispersion, to seriously affect the electric conductivity of lithium ion battery and the efficiency for charge-discharge of battery.For example,
Graphene is after being added directly to positive and negative pole material, although graphene is face contact conductive agent, electric conductivity is good, its to point
It dissipates and requires excessively high, and it is caused to disperse unevenness in the electrodes, to seriously affect the property such as efficiency for charge-discharge of lithium ion battery
Energy.
In order to overcome the conductive agent to be uniformly dispersed or be difficult to the problems such as dispersing, patent 201410828734.9 proposes use
Inorganic dispersant carries out adsorption treatment to graphene surface, is easy to happen asking for reunion to improve graphene in electrocondution slurry
Topic, although handling graphene the reunion that can be reduced between graphene using inorganic dispersant, can not still solve
Certainly its uniformity and stability problem.
Therefore the graphene and graphene uniform dispersion and the stable conductive paste of dispersion of a kind of high quality how to be researched and developed
Material is the emphasis that the present invention inquires into.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of graphene of high quality and graphene uniform dispersion and disperse
Efficient, high dispersive graphene conductive slurry the preparation method of stable system.
In order to solve the above technical problems, the technical solution of the present invention is as follows: a kind of efficient, high dispersive graphene conductive slurry
Preparation method, innovative point are: being mixed by material --- high speed and high pressure grinding ---, and three steps of ultrasonic emulsification are constituted, specific to walk
It is rapid as follows:
Step 1: material mixing: by raw graphite, solvent and dispersing agent are stirred at 20-50 DEG C by formula rate addition batching kettle
1-3h is mixed, graphite mixed liquor is made, wherein the graphite quality concentration of the graphite mixed liquor is 0.1~8%, and dispersing agent quality is dense
Degree is 0.01~0.5%, and rest part is solvent；
Step 2: high speed and high pressure grinding: being delivered to high speed grinding unit for above-mentioned graphite mixed liquor with the flow of 0.5~5T/h,
Material enters pans after high speed grinding, then is transported in high pressure abrasive machine and handles；
Step 3: ultrasonic emulsification: being delivered to ultrasonic sound appratus group by the flow pump of 0.5~5T/h for the material after high pressure abrasive,
Material after ultrasound removing enters emulsifier unit and carries out 1~10h of emulsification treatment, keeps graphene distribution more uniform, after emulsification i.e.
Graphene conductive slurry finished product is obtained, finished pot storage is delivered to.
Further, it is 250~500 mesh, the graphite that content is 99.99% that raw graphite, which selects mesh number, in the step 1.
Further, solvent is selected from water, ammonium hydroxide, ethyl alcohol, isopropanol, acetone, butanol, toluene, second two in the step 1
Alcohol, N- methyl pyrrolidone, dimethylformamide, tetrahydrofuran, dimethyl acetamide, o-dichlorohenzene, acetonitrile, 1,2- dichloro
One or more combinations of ethane.
Further, in the step 1 powder be BYK-163, BYK-161, sodium carboxymethylcellulose, polyethylene glycol,
Cetyl ammonium bromide, dodecyl sodium sulfate, neopelex, polytetrafluoroethylene (PTFE), butadiene-styrene rubber, tween and
The combination of TritonX-100 one or more.
Further, the step 2 high speed grinding unit is composed in series by the high-speed grinder of 2~12 11KW, and
The pressure of high pressure abrasive machine is set as 800~1200KG.
Further, the material after the step 2 high speed grinding passes through one or both of impeller pump, diaphragm pump
It beats to pans.
Further, ultrasonic sound appratus group is made of 6~20 ultrasonic sound appratus in the step 3, ultrasonic time be 1~
10h。
The present invention has the advantages that
(1) efficient, high dispersive graphene conductive slurry preparation method of the invention, prepares graphene conductive slurry using one-step method
Material, simplifies and first prepares the complex techniques process that graphene prepares electrocondution slurry again；In addition, using high speed grinding, high pressure abrasive,
Ultrasound, emulsification method prepare graphene conductive slurry, the graphene made quality with higher, electrocondution slurry have compared with
High dispersibility gives full play to its excellent electric conductivity；The conductive height compared with conventional conductive slurry, the service life is long, again
Measure low advantage；
(2) efficient, high dispersive graphene conductive slurry preparation method of the invention, this method adapt to use different solvents, belong to object
Reason method does not destroy the structure of graphene, can obtain high-quality, flawless graphene；Meanwhile this method use high speed,
The mechanical dispersion effect of high pressure abrasive, ultrasonic wave, strengthens the stripping process of graphite, to realize the height of graphene conductive slurry
Effect, quickly preparation.
Specific embodiment
The following examples can make professional and technical personnel that the present invention be more fully understood, but therefore not send out this
It is bright to be limited among the embodiment described range.
Embodiment 1
Step 1: the formula of graphene conductive slurry is as follows:
NMP(N- methyl pyrrolidone) 1000KG
Graphite (320 mesh) 50KG(content 99.99%)
Dispersing agent (BYK-163) 2.5KG
Above-mentioned ingredient is added in the batching kettle of stainless steel material, stirs 1h in 150 turns/h at 50 DEG C, be sufficiently mixed material
It is even.
Step 2: the above-mentioned material mixed is delivered in high speed grinding unit, and the flow control of material is ground in 2T/h
Grinding machine group is composed in series by the high-speed grinder of 6 11KW, and the material after high speed grinding is beaten by impeller pump to pans.It is intermediate
The material of tank is transported in high pressure abrasive machine with the flow of 2T/h and is handled, and the pressure of high pressure abrasive machine is controlled in 1000KG.
Step 3: the material after high pressure abrasive is delivered to ultrasonic sound appratus group by pump with 2T/h flow and carries out ultrasonic wave removing
2h, ultrasonic sound appratus group are composed in series by 16 ultrasonoscopes.Material after ultrasound removing enters emulsifier unit and carries out processing 3h, makes
Graphene distribution is more uniform.Graphene conductive slurry finished product is obtained after emulsification, is delivered to finished pot storage.
Embodiment 2
Step 1: the formula of graphene conductive slurry is as follows:
DMF(dimethylformamide) 1200KG
Graphite (300 mesh) 50KG(content 99.99%)
Dispersing agent (sodium carboxymethylcellulose) 2.5KG
Above-mentioned ingredient is added in the batching kettle of stainless steel material, stirs 2h in 150 turns/h at 20 DEG C, be sufficiently mixed material
It is even.
Step 2: the above-mentioned material mixed is delivered in high speed grinding unit, and the flow control of material is ground in 1T/h
Grinding machine group is composed in series by the high-speed grinder of 3 11KW, and the material after high speed grinding is beaten by impeller pump to pans.It is intermediate
The material of tank is transported in high pressure abrasive machine with the flow of 1T/h and is handled, and the pressure of high pressure abrasive machine is controlled in 800KG.
Step 3: the material after high pressure abrasive is delivered to ultrasonic sound appratus group by pump with 1T/h flow and carries out ultrasonic wave removing
2h, ultrasonic sound appratus group are composed in series by 8 ultrasonoscopes.Material after ultrasound removing enters emulsifier unit and carries out processing 2h, makes
Graphene distribution is more uniform.Graphene conductive slurry finished product is obtained after emulsification, is delivered to finished pot storage.
Embodiment 3
Step 1: the formula of graphene conductive slurry is as follows:
Ethylene glycol 1000KG
Graphite (400 mesh) 50KG(content 99.99%)
Dispersing agent (BYK-161) 2.5KG
Above-mentioned ingredient is added in the batching kettle of stainless steel material, stirs 1h in 150 turns/h at 25 DEG C, be sufficiently mixed material
It is even.
Step 2: the above-mentioned material mixed is delivered in high speed grinding unit, and the flow control of material is ground in 2T/h
Grinding machine group is composed in series by the high-speed grinder of 6 11KW, and the material after high speed grinding is beaten by impeller pump to pans.It is intermediate
The material of tank is transported in high pressure abrasive machine with the flow of 2T/h and is handled, and the pressure of high pressure abrasive machine is controlled in 1200KG.
Step 3: the material after high pressure abrasive is delivered to ultrasonic sound appratus group by pump with 2T/h flow and carries out ultrasonic wave removing
2h, ultrasonic sound appratus group are composed in series by 16 ultrasonoscopes.Material after ultrasound removing enters emulsifier unit and carries out processing 2h, makes
Graphene distribution is more uniform.Graphene conductive slurry finished product is obtained after emulsification, is delivered to finished pot storage.
Embodiment 4
Step 1: the formula of graphene conductive slurry is as follows:
NMP(N- methyl pyrrolidone) 1200KG
Graphite (250 mesh) 50KG(content 99.99%)
Dispersing agent (cetyl ammonium bromide) 2.5KG
Above-mentioned ingredient is added in the batching kettle of stainless steel material, stirs 3h in 150 turns/h at 40 DEG C, be sufficiently mixed material
It is even.
Step 2: the above-mentioned material mixed is delivered in high speed grinding unit, and the flow control of material is ground in 3T/h
Grinding machine group is composed in series by the high-speed grinder of 8 11KW, and the material after high speed grinding is beaten by impeller pump to pans.It is intermediate
The material of tank is transported in high pressure abrasive machine with the flow of 3T/h and is handled, and the pressure of high pressure abrasive machine is controlled in 1200KG.
Step 3: the material after high pressure abrasive is delivered to ultrasonic sound appratus group by pump with 3T/h flow and carries out ultrasonic wave removing
5h, ultrasonic sound appratus group are composed in series by 18 ultrasonoscopes.Material after ultrasound removing enters emulsifier unit and carries out processing 6h, makes
Graphene distribution is more uniform.Graphene conductive slurry finished product is obtained after emulsification, is delivered to finished pot storage.
Embodiment 5
Step 1: the formula of graphene conductive slurry is as follows:
Acetonitrile 700KG
Graphite (320 mesh) 50KG(content 99.99%)
Dispersing agent (polyethylene glycol) 2.5KG
Above-mentioned ingredient is added in the batching kettle of stainless steel material, stirs 2h in 150 turns/h at 20 DEG C, be sufficiently mixed material
It is even.
Step 2: the above-mentioned material mixed is delivered in high speed grinding unit, and the flow control of material is ground in 2T/h
Grinding machine group is composed in series by the high-speed grinder of 6 11KW, and the material after high speed grinding is beaten by impeller pump to pans.It is intermediate
The material of tank is transported in high pressure abrasive machine with the flow of 2T/h and is handled, and the pressure of high pressure abrasive machine is controlled in 800KG.
Step 3: the material after high pressure abrasive is delivered to ultrasonic sound appratus group by pump with 2T/h flow and carries out ultrasonic wave removing
3h, ultrasonic sound appratus group are composed in series by 16 ultrasonoscopes.Material after ultrasound removing enters emulsifier unit and carries out processing 2h, makes
Graphene distribution is more uniform.Graphene conductive slurry finished product is obtained after emulsification, is delivered to finished pot storage.
Embodiment 6
Step 1: the formula of graphene conductive slurry is as follows:
Butanol 800KG
Graphite (450 mesh) 50KG(content 99.99%)
Dispersing agent (polytetrafluoroethylene (PTFE)) 2.5KG
Above-mentioned ingredient is added in the batching kettle of stainless steel material, stirs 1h in 150 turns/h at 25 DEG C, be sufficiently mixed material
It is even.
Step 2: the above-mentioned material mixed is delivered in high speed grinding unit, and the flow control of material is ground in 1T/h
Grinding machine group is composed in series by the high-speed grinder of 4 11KW, and the material after high speed grinding is beaten by impeller pump to pans.It is intermediate
The material of tank is transported in high pressure abrasive machine with the flow of 1T/h and is handled, and the pressure of high pressure abrasive machine is controlled in 1000KG.
Step 3: the material after high pressure abrasive is delivered to ultrasonic sound appratus group by pump with 1T/h flow and carries out ultrasonic wave removing
2h, ultrasonic sound appratus group are composed in series by 10 ultrasonoscopes.Material after ultrasound removing enters emulsifier unit and carries out processing 3h, makes
Graphene distribution is more uniform.Graphene conductive slurry finished product is obtained after emulsification, is delivered to finished pot storage.
Comparative example 1: using carbon black as conductive agent
The conductive agent of the graphene conductive agent of embodiment 1-6 and comparative example 1 is fabricated to flexible packing lithium ion battery,
Cycle performance test is carried out, as a result as follows:
| Project | The internal resistance of cell/m Ω | 2-3.6V, 1C, 500 circulation volume conservation rates | Conductivity additive amount/% | First charge discharge efficiency/% |
| Embodiment 1 | 12 | 92 | 50 | 92 |
| Embodiment 2 | 13 | 91 | 52 | 90 |
| Embodiment 3 | 15 | 88 | 55 | 87 |
| Embodiment 4 | 13 | 92 | 53 | 90 |
| Embodiment 5 | 14 | 90 | 54 | 88 |
| Embodiment 6 | 12 | 91 | 50 | 91 |
| Comparative example | 35 | 60 | 100 | 68 |
As can be seen from the above table, the present invention uses graphene conductive agent, using the excellent electric conductivity of graphene, reduces in battery
Resistance improves battery cycle life；Dosage of the graphene conductive agent when preparing lithium ion battery is only existing conductive agent dosage
50-55% saves cost, so that lithium ion battery is more competitive.
Basic principles and main features and advantages of the present invention of the invention have been shown and described above.The skill of the industry
Art personnel it should be appreciated that the present invention is not limited to the above embodiments, the above embodiments and description only describe
The principle of the present invention, without departing from the spirit and scope of the present invention, various changes and improvements may be made to the invention, these
Changes and improvements all fall within the protetion scope of the claimed invention.The claimed scope of the invention by appended claims and
Its equivalent thereof.
Claims (7)
1. a kind of efficient, high dispersive graphene conductive slurry preparation method, it is characterised in that: mixed by material --- high speed is high
Pressure grinding --- three steps of ultrasonic emulsification are constituted, the specific steps are as follows:
Step 1: material mixing: by raw graphite, solvent and dispersing agent are stirred at 20-50 DEG C by formula rate addition batching kettle
1-3h is mixed, graphite mixed liquor is made, wherein the graphite quality concentration of the graphite mixed liquor is 0.1~8%, and dispersing agent quality is dense
Degree is 0.01~0.5%, and rest part is solvent；
Step 2: high speed and high pressure grinding: being delivered to high speed grinding unit for above-mentioned graphite mixed liquor with the flow of 0.5~5T/h,
Material enters pans after high speed grinding, then is transported in high pressure abrasive machine and handles；
Step 3: ultrasonic emulsification: being delivered to ultrasonic sound appratus group by the flow pump of 0.5~5T/h for the material after high pressure abrasive,
Material after ultrasound removing enters emulsifier unit and carries out 1~10h of emulsification treatment, keeps graphene distribution more uniform, after emulsification i.e.
Graphene conductive slurry finished product is obtained, finished pot storage is delivered to.
2. efficient, high dispersive graphene conductive slurry preparation method according to claim 1, it is characterised in that: described
It is 250~500 mesh, the graphite that content is 99.99% that raw graphite, which selects mesh number, in step 1.
3. efficient, high dispersive graphene conductive slurry preparation method according to claim 1, it is characterised in that: described
Solvent is selected from water, ammonium hydroxide, ethyl alcohol, isopropanol, acetone, butanol, toluene, ethylene glycol, N- methyl pyrrolidone, two in step 1
Methylformamide, tetrahydrofuran, dimethyl acetamide, one or more groups of o-dichlorohenzene, acetonitrile, 1,2- dichloroethanes
It closes.
4. efficient, high dispersive graphene conductive slurry preparation method according to claim 1, it is characterised in that: described
Powder is BYK-163, BYK-161, sodium carboxymethylcellulose, polyethylene glycol, cetyl ammonium bromide, dodecane in step 1
Base sodium sulfonate, neopelex, polytetrafluoroethylene (PTFE), butadiene-styrene rubber, tween and TritonX-100 are one or more kinds of
Combination.
5. efficient, high dispersive graphene conductive slurry preparation method according to claim 1, it is characterised in that: described
Step 2 high speed grinding unit is composed in series by the high-speed grinder of 2~12 11KW, and the pressure setting of high pressure abrasive machine
For 800~1200KG.
6. efficient, high dispersive graphene conductive slurry preparation method according to claim 1, it is characterised in that: described
Material after the grinding of step 2 high speed is beaten by one or both of impeller pump, diaphragm pump to pans.
7. efficient, high dispersive graphene conductive slurry preparation method according to claim 1, it is characterised in that: described
Ultrasonic sound appratus group is made of 6~20 ultrasonic sound appratus in step 3, and ultrasonic time is 1~10h.
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| CN108373293A (en) * | 2018-03-29 | 2018-08-07 | 广东盛达穗南环保科技有限公司 | Damping sound-absorbing mixture and its production method for road noise barrier |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103922330A (en) * | 2014-04-28 | 2014-07-16 | 南京新月材料科技有限公司 | Method for preparing graphene powder by using dry process |
| CN105086905A (en) * | 2015-09-22 | 2015-11-25 | 黑龙江大学 | Preparation method of graphene-enhanced epoxy resin adhesive |
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Application publication date: 20181221 |
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| RJ01 | Rejection of invention patent application after publication |