CN109455707A - A kind of graphene slurry and preparation method thereof of the grinding aid containing dispersion - Google Patents
A kind of graphene slurry and preparation method thereof of the grinding aid containing dispersion Download PDFInfo
- Publication number
- CN109455707A CN109455707A CN201811606958.XA CN201811606958A CN109455707A CN 109455707 A CN109455707 A CN 109455707A CN 201811606958 A CN201811606958 A CN 201811606958A CN 109455707 A CN109455707 A CN 109455707A
- Authority
- CN
- China
- Prior art keywords
- dispersion
- grinding aid
- carbon black
- graphene
- slurry
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- 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
-
- 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
- C01B2204/32—Size or surface area
Abstract
The present invention provides a kind of graphene slurry and preparation method thereof of grinding aid containing dispersion, and the graphene slurry is made of graphene, dispersion grinding aid and solvent；Wherein, the dispersion grinding aid is carbon black particle, is less than 300nm by the partial size D50 of the carbon black particle of laser particle analyzer test.When preparing the graphene slurry; dispersion grinding aid can reduce the difficulty of expanded graphite grinding removing; dispersion grinding aid between expanded graphite lamella is easy to slide and reducing slurry viscosity improves rheological characteristic; it improves and efficiency is sanded; the physical barrier dispersing agent that carbon black particle is also used as graphene in slurry simultaneously is used, the graphene slurry good conductivity prepared.
Description
Technical field
The invention belongs to graphene slurry fields, and in particular to a kind of containing the graphene slurry for dispersing grinding aid and its preparation
Method.
Background technique
Graphene is a kind of thin layer two-dimension nano materials, has high-specific surface area, high surface energy, and piece interlayer has strong model moral
Hua Li and big pi bond conjugation, it is easy to reunite and return folded.When liquid phase stripping method prepares graphene, separate in order to prevent
The graphene come occur can not reverse back it is folded, dispersing agent must generally be added to prevent from reuniting and return folded.
The dispersing agent usually added in the industry now is the surfactant or organic polymer of organic, from certain meaning
For upper, this kind of organic dispersing agent is a kind of impurity, will affect the performance of graphene performance, especially electric conductivity.Such as:
(1) surfactant, such as: conventional dispersant polyvinyl alcohol that patent CN201610001211.6 is used, gelatin, TWEEN Series,
Span series；(2) the coated barrier of polymer, such as: adding PVDF in patent CN201510962558.2；(3) π-π coupling dispersion
Agent, such as: the electroactive high molecular π-π compound of the unit containing oligomer of phenylamine is added in patent CN201510770154.3.
The dispersing agent that another kind often adds in the industry is small size inorganic dispersing agent, is substantially a kind of physical barrier agent,
Such as add carbon black, carbon pipe.For example small size barrier is added in patent CN201410828853.4: acetylene black, Ketjen black, carbon are received
Mitron.But it due to the more difficult matching of the size of acetylene black, Ketjen black, carbon nanotube and graphene, is in contact with each other a little less, contact area
It is small to cause binding force weak, so also needing addition dispersing agent and adhesive, these will affect most other than adding small size barrier
Whole electric conductivity.Faced with this situation, it is badly in need of finding the dispersing agent that compatible with graphene system, additive amount is few and does not influence conduction.
Liquid phase stripping method using expanded graphite as raw material to prepare graphene when, it is main that two kinds of effects: expanded graphite occur
Removing and graphite flake diameter reduce between lamella, industrially commonly use sand mill now to remove and be crushed.Technological difficulties therein are
Expandable graphite sheet intensity is very high, and non-breakable and removing needs to remove grinding very to reach the granularity and lamellar spacing of requirement
Long time and very high to equipment requirement, it will lead to the high popularization and application for influencing graphene slurry of production cost in this way.
Summary of the invention
In view of the deficiencies of the prior art, the graphene slurry and its system of the grinding aid containing dispersion of mode is implemented as follows in the present invention
Preparation Method:
A kind of graphene slurry of the grinding aid containing dispersion, is made of graphene, dispersion grinding aid and solvent；Wherein, described
Dispersion grinding aid is carbon black particle, is less than 300nm by the partial size D50 of the carbon black particle of laser particle analyzer test.
Optionally, the partial size D50 for the carbon black particle that the dispersion grinding aid is tested by laser particle analyzer is less than
200nm。
Optionally, the dispersion grinding aid is the broken body of carbon black primary structure body, passes through high pressure by the dispersion liquid of carbon black
Homogeneous crusher machine is made.
Optionally, dispersion grinding aid and graphene mass ratio are 1:200~1:2.
Optionally, dispersion grinding aid and graphene mass ratio are 1:100~1:7.
Optionally, solvent is the combination of organic solvent, any one or two kinds in resin.
Optionally, the pole piece resistivity of the graphene conductive slurry is 2.0~7.5 Ω cm.
A kind of preparation method of the graphene slurry of the grinding aid containing dispersion, which is characterized in that first carbon black dispersion
In solvent, the dispersion liquid of carbon black is obtained；The dispersion liquid of carbon black is carried out homogeneous with high pressure homogenizer to be crushed, is obtained broken containing carbon black
The dispersion liquid of grain；Then the dispersion liquid of carbon black, expanded graphite and solvent are carried out dispersion mixing with high speed disperser, is premixed
Material；Premix is finally put into progress liquid phase removing in sand mill, obtains the graphene slurry of the grinding aid containing dispersion.
Optionally, when liquid phase removes expanded graphite, sand mill linear velocity is greater than 8m/s；The homogenization pressure of high pressure homogenizer
Greater than 60MPa.
Optionally, the expansion multiplying power of expanded graphite is more than or equal to 200 times.
Compared with prior art, the graphene slurry of the grinding aid provided by the invention containing dispersion is by graphene, dispersion grinding aid
Three kinds of groups of agent and solvent are grouped as, and due to the organic dispersing agent without insulation in slurry system, the dispersion grinding aid is carbon black
Particle, it is also conductive since the carbon black particle is by the broken preparation of physics, disperse that grinding aid additive amount itself is few and energy
Conduction, so slurry good conductivity obtained.The physical barrier that carbon black particle is also used as graphene in slurry simultaneously is dispersed
Agent is used, and is prevented graphene sheet layer from returning folded, is played the role of stable dispersion.When preparing the graphene slurry, disperse grinding aid
The difficulty of expanded graphite grinding removing can be reduced, the dispersion grinding aid between expanded graphite lamella is easy to slide and reduce slurry
Expect that viscosity improves rheological characteristic, improves and efficiency is sanded.
Detailed description of the invention
Fig. 1 is the particle diameter distribution of embodiment 1 and 1 carbon black of comparative example under the conditions of by different disposal.
Fig. 2 is the graphene pattern of the addition dispersion grinding aid of the embodiment of the present invention 2.
Fig. 3 is the graphene powder SEM picture of 4 adsorption carbon black of comparative example.
Specific embodiment
Below by specific embodiment, the present invention is described in further detail, but the present invention is not limited to tool below
Body embodiment.
The graphene slurry of the grinding aid containing dispersion of the specific embodiment of the invention, by graphene, dispersion grinding aid and molten
Three kinds of groups of agent are grouped as, wherein the dispersion grinding aid is carbon black particle, by the carbon black particle of laser particle analyzer test
Partial size D50 is less than 300nm.Through research, the inventor has found that the constituent structure of carbon black particle of the invention connects very much with graphite
Closely, and it is small-sized, it is easy to it is adsorbed on expanded graphite surface, reduces the surface free energy of graphene, meanwhile, it is described further
Carbon black particle is the broken body of carbon black primary structure body, and the very sharp crack defect that can extend expanded graphite in edge is improved and is sanded
Easy degree；And the carbon black particle is compared with the nano-particle carbon (subsphaeroidal no corner angle) of known low structure, although
May be similar on size, but the present invention is the broken body of carbon black primary structure body, the corner angle for possessing carbon black can be more advantageous
In grinding aid；It is broken graphite microcrystal on carbon black particle is microcosmic, phorogenesis can be played, slurry viscosity can be reduced, improves rheological characteristic,
It improves and efficiency is sanded；Carbon black broken particle is also used as expanded graphite simultaneously and the physical barrier dispersing agent of graphene is used, and prevents
Graphene sheet layer returns folded.Organic dispersing agent can be added to prevent from settling in usual graphene conductive slurry, organic dispersing agent can be broken
Its bad electric conductivity, and carbon black particle of the invention is conductive, will not reduce the electric conductivity of graphene conductive slurry.Further
In order to meet more preferable grinding aid, 200nm is less than by the partial size D50 of the carbon black particle of laser particle analyzer test, it is usually described
The partial size of carbon black particle can all be more than or equal to the carbon black primary partical diameter.The partial size D50 refers to cumulative particle sizes distribution hundred
Score reaches partial size corresponding when 50%, and the particle greater than the partial size accounts for 50%, and the particle less than the partial size also accounts for
50%, D50 are also meso-position radius or median particle diameter, and D50 is commonly used to indicate the average particle size of powder.
The graphene slurry of the grinding aid containing dispersion of the specific embodiment of the invention, the dispersion grinding aid are that carbon black is primary
The broken body of structural body is made by the dispersion liquid of carbon black by high-pressure homogeneous crusher machine.In general, the dispersion grinding aid be comprising
The dispersion liquid of the carbon black particle of the solvent, in the dispersion liquid of the carbon black particle, the solid content of the carbon black particle is
0.1~10wt%, preferably 1~8wt%, specifically for example can be 1wt%, 2wt%, 3wt%, 4wt%, 5wt%, 6wt%,
7wt% etc..
The graphene slurry of the grinding aid containing dispersion of the specific embodiment of the invention, on additive amount, dispersion grinding aid (admittedly contain
Amount) it with expanded graphite or with the mass ratio of graphene is 1:200~1:2.In view of the electric conductivity of carbon black particle is not so good as graphene,
Having can guarantee dispersion stabilization and under the premise of have grind -aiding effect, as far as possible less plus, it is very few and grinding aid and dispersion is not achieved
Effect, preferred mass ratio are 1:100~1:7, are further preferably 1:50~1:20, specifically for example, 1:20,1:21,1:22,1:
23,1:24,1:25,1:27,1:28,1:29,1:30,1:40,1:50 etc..
The specific embodiment of the invention containing dispersion grinding aid graphene slurry, the solvent can for organic solvent,
The combination of any one or two kinds in resin, preferably organic solvent, the organic solvent includes but is not limited to: NMP (N- first
Base pyrrolidones), DMF (n,N-Dimethylformamide), n,N-dimethylacetamide, dimethyl sulfoxide, ethyl alcohol, isopropanol, benzene
Methanol, ethyl acetate, toluene, dimethylbenzene, tetrahydrofuran etc., further preferred NMP, DMF.In the graphene slurry, admittedly contain
Amount, i.e., the content of graphene and grinding aid be 0.1~10wt%, preferably 1~8wt%, specifically for example can be 1wt%,
2wt%, 3wt%, 4wt%, 5wt%, 6wt%, 7wt% etc..
The graphene slurry of the grinding aid containing dispersion of the specific embodiment of the invention, the pole piece of the graphene conductive slurry
Resistivity is 2.0~7.5 Ω cm, specifically for example can be 3 Ω cm, 3.5 Ω cm, 4 Ω cm, 4.5 Ω cm, 5
Ω cm, 5.5 Ω cm, 6 Ω cm, 6.5 Ω cm, 7 Ω cm etc..
The graphene slurry of the grinding aid containing dispersion of the specific embodiment of the invention, the carbon black is by acetylene carbon black, by-product
One or more of compositions of carbon black and furnace black.
The preparation method of the graphene slurry of the grinding aid of the present invention containing dispersion, as an example, method is as follows and not
It is only limitted to this.First carbon black dispersion in solvent, the dispersion liquid of carbon black is obtained；The dispersion liquid high pressure homogenizer of carbon black into
Row homogeneous is broken, obtains the dispersion liquid of the particle containing carbon black；Then the dispersion liquid of carbon black, expanded graphite and solvent high speed dispersion
Machine carries out dispersion mixing, obtains premix；Premix is finally put into progress liquid phase removing in sand mill, obtains the grinding aid containing dispersion
The graphene slurry of agent.After sand milling, the dispersion grinding aid and expanded graphite or graphene film be by Van der Waals force and
π-π active force attracts each other, and can closely attach in expanded graphite and graphene surface, no longer needs to addition organic dispersing agent.
The preparation method of the graphene slurry of the grinding aid of the present invention containing dispersion, the sand mill linear velocity are greater than 8m/
S, preferably greater than or equal to 12m/s.
The preparation method of the graphene slurry of the grinding aid of the present invention containing dispersion, carbon black is added in solvent, with dispersion
Disk is pre-dispersed, falls bulky grain with screen filtration, obtains carbon black dispersion liquid, and high pressure homogenizer then is added in the carbon black dispersion liquid
In, homogeneous is broken.Under the conditions of carbon black manufacturing process high temperature, adjacent primary partical generates simultaneously, is mutually melt into chain, and occupy three
Dimension space, this is referred to as primary structure, is also primary structure.Primary structure is generally difficult to destroy, and what the present invention initiated utilizes height
Pressure homogenizer can be crushed it, and carbon black is molten to get together to form " grape cluster " shape aggregation in order to smash, and need using using
Homogenization pressure to the void effect of high pressure homogenizer and the shearing force of turbulent flow, the high pressure homogenizer is greater than 60MPa, preferably greatly
In being equal to 80Mpa, further preferably greater than it is equal to 100Mpa.The dispersion of high pressure homogenizer putty in order to prevent, carbon black needs
Sieving removes big aggregate, and the mesh number of the sieve is 50 mesh or more, more than preferably 80 mesh.
It is described further below by way of specific embodiment.
Raw material explanation:
Carbon black: it is purchased from Shanghai Hai Yi scientific & trading Co., Ltd., the production of You Yirui stone company, model is Super P Li
Expanded graphite: be purchased from one sail graphite Co., Ltd of Shanghai, 400 times of expansion multiplying power, 300 microns of partial size.
NMP: it is purchased from Jinan Lian Cheng Chemical Co., Ltd., purity is electronic pure.
Test specification:
Viscosity test: it is tested using the DV2T-RV type viscosimeter that Brookfield is produced.Rotor is No. 21, test
When setting value between be divided into 5 seconds, the time be 1 minute, using the average viscosity of last three points as the viscosity number of institute's sample.Test
When shearing rate (shear rate) be set as 10S-1.Temperature when test is controlled at 25 ± 1 DEG C.
The test of D50 partial size: test equipment is Dandong Bai Te laser particle analyzer S2600, and NMP does mobile phase, and when test reflects
Rate is real part 1.8 and imaginary part 0.7, after scanning mobile phase background, takes 1 droplet slurry sample to instill sample cell, test with small dropper
The preceding ultrasonic machine built in laser particle analyzer is ultrasonically treated 30 seconds, and follow-on test is averaged.
Pole piece resistivity measurement: the graphene composite mortar is used in lithium ion battery ternary system material, according to three
523 active material T31R of member, Kynoar HSV900, containing dispersion grinding aid graphene slurry conductive agent (in terms of solid content)
Mass ratio be 100:1.5:1.5, be made just after stirring 2 hours by adding NMP adjustment solid containing to 72%, closing 600rpm in pulp grinder
Pole slurry is coated on the slurry of mixing on PET film with coating machine, 90 degree drying 1 hour after obtain anode pole piece.By positive pole
Piece (PET film) is cut into 5cmx5cm square, pole piece thickness is measured using micrometer caliper, using Suzhou lattice ST2258C type four
Probe resistance rate tester test pole sheet resistivity.
SEM test: containing dispersion grinding aid 200ml graphene slurry with solvent filter filter out the inside solvent
NMP, then plus deionized water 3000ml it is repeated multiple times flushing displace NMP, obtain graphene aqueous slurry 200ml, ultrasonic disperse 1
Minute, graphene aqueous slurry is then frozen into rapidly thin piece, then be freeze-dried to obtain graphene powder with freeze dryer, finally handle
Graphene powder, which is put into field emission scanning electron microscope, tests SEM.
Sedimentation stability test: it takes 150g graphene slurry to be put into the Clear glass bottles and jars that volume is 150ml, seals room temperature
Under static placement, with week be interval observation sedimentation situation, test the solid content of 1/3 eminence slurry of chaotropic face under different time of repose
Value, it is initially solid when differing 10% containing value when test value is with just preparation, it is believed that slurry has settled, which is sedimentation stability
Time.
Embodiment
Embodiment 1
50g carbon black Super P Li is added in 950gNMP, with the pre-dispersed 15min of dispersion impeller 1500rpm, after 80 mesh
Stainless steel sieve, obtains carbon black dispersion liquid.Then carbon black dispersion liquid is added in high-pressure homogeneous, homogenization pressure 120MPa, homogeneous 1
Time, obtain dispersion grinding aid 1；Carbon black dispersion liquid is put into high pressure homogenizer, homogenization pressure 100MPa, homogeneous 1 time, is obtained
Disperse grinding aid 2；Carbon black dispersion liquid is put into high pressure homogenizer, homogenization pressure 80MPa, homogeneous 1 time, obtains dispersion grinding aid
Agent 3.Carbon black dispersion and 3 obtained dispersion grinding aids are tested partial size, the result is shown in Figure 1 and table 1 with laser particle analyzer respectively.
Embodiment 2
The dispersion of 16g obtained in embodiment 1 grinding aid 1 (by solid containing calculation), the expansion stone that 384g expansion multiplying power is 400 times
Ink, 7280g solvent NMP carry out dispersion with high speed disperser 2500RPM and mix 1 hour, obtain premix；Then premix is put
Enter to carry out being sanded in sand mill liquid phase removing, sand mill linear velocity is 12m/s, and sand mill zirconium pearl diameter is 1 millimeter, and the time is sanded
It is 5 hours, obtains the graphene slurry of the grinding aid containing dispersion.The granularity and viscosity of 2 hours intermediate state materials is sanded in detection.
Viscosity test, testing graininess and pole piece resistivity measurement are carried out to obtained graphene slurry, the results are shown in Table 2；Washing freeze-drying is surveyed
SEM is tried, as a result sees Fig. 2.
Embodiment 3
Dispersion grinding aid used in embodiment 2 is changed into dispersion grinding aid 2, other conditions are constant.
Embodiment 4
Dispersion grinding aid used in embodiment 2 is changed into dispersion grinding aid 3, other conditions are constant.
Embodiment 5
The additive amount of dispersion grinding aid 1 used in embodiment 2 is changed to 4g (by solid containing calculation), expansion multiplying power 400
The additive amount of expanded graphite again is changed to 396g, and other conditions are constant.
Embodiment 6
The additive amount of dispersion grinding aid 1 used in embodiment 2 is changed to 50g (by solid containing calculation), expansion multiplying power 400
The additive amount of expanded graphite again is changed to 350g, and other conditions are constant.
Comparative example
Comparative example 1
400g carbon black Super P Li is added in 7600gNMP, it is small to carry out dispersion mixing 1 with high speed disperser 2500RPM
When, obtain carbon black dispersion；Then carbon black dispersion is put into sand mill and be sanded liquid phase removing, sand mill linear velocity is
12m/s, sand mill zirconium pearl diameter are 1 millimeter, and it is 2 hours that the time, which is sanded, obtain carbon black and material is sanded.Grain is tested with laser particle analyzer
Diameter, the result is shown in Figure 1 and table 1.
Comparative example 2
400g expansion multiplying power be 400 times expanded graphite, 7600g solvent NMP divided with high speed disperser 2500RPM
It dissipates and mixes 1 hour, obtain premix；Then premix is put into sand mill and be sanded liquid phase removing, sand mill linear velocity
For 12m/s, sand mill zirconium pearl diameter is 1 millimeter, and it is 5 hours that the time, which is sanded, obtains carbon black and graphene compound size.Detect sand
The granularity and viscosity of 2 hours intermediate state materials of mill.Viscosity test, testing graininess and pole piece are carried out to obtained compound size
Resistivity the results are shown in Table 2.
Comparative example 3
16g toner body Super P Li, the expanded graphite that 384g expansion multiplying power is 400 times, 7600g solvent NMP high
Fast dispersion machine 2500RPM carries out dispersion and mixes 1 hour, obtains premix；Then premix is put into sand mill and is sanded
Liquid phase removing, sand mill linear velocity be 12m/s, sand mill zirconium pearl diameter be 1 millimeter, be sanded the time be 5 hours, obtain carbon black with
Graphene compound size.The granularity and viscosity of 2 hours intermediate state materials is sanded in detection.Obtained compound size is glued
Degree test, testing graininess and pole piece resistivity, the results are shown in Table 2.
Comparative example 4
With reference to CN20141082885,30g graphene and 10g carbon black is taken to stir ultrasound 1h in ethanol, after mixing 80
DEG C drying, obtains the graphene powder of adsorption carbon black, tests SEM, as a result see Fig. 3.16g dispersing agent PVP K30 powder,
The graphene powder of 384g adsorption carbon black adds NMP to be diluted to the 8kg slurry containing 5% admittedly, and is put into sand mill and carries out sand
Grinding fluid is mutually removed, and sand mill linear velocity is 12m/s, and sand mill zirconium pearl diameter is 1 millimeter, and it is 5 hours that the time, which is sanded, obtains carbon black
With graphene compound size.The granularity and viscosity of 2 hours intermediate state materials is sanded in detection.Obtained compound size is carried out
Viscosity test, testing graininess and pole piece resistivity, the results are shown in Table 2.
Comparative example 5
16g dispersing agent PVP K30 powder, the expanded graphite that 384g expansion multiplying power is 400 times, 7600g solvent NMP high speed
Dispersion machine 2500RPM carries out dispersion and mixes 1 hour, obtains premix；Then premix is put into sand mill and carries out sand milling liquid
It mutually removes, sand mill linear velocity is 12m/s, and sand mill zirconium pearl diameter is 1 millimeter, and it is 5 hours that the time, which is sanded, obtains carbon black and stone
Black alkene compound size.The granularity and viscosity of 2 hours intermediate state materials is sanded in detection.Viscosity is carried out to obtained compound size
Test, testing graininess and pole piece resistivity, the results are shown in Table 3.
Table 1
Table 2
According to Fig. 1 and table 1, it can be seen that conventional dispersion and sand milling cannot be crushed carbon black primary structure body.And high pressure is equal
Matter function smashes the primary structure body of carbon black, obtains the particle of carbon black, i.e. carbon black primary partical.
The D50 for dispersing grinding aid 1, dispersion grinding aid 2, dispersion grinding aid 3 obtained according to 1 embodiment 1 of table is it is found that difference
The D50 of the carbon black particle obtained under homogenization pressure be it is different, when homogenization pressure be greater than 80MPa when, D50 can be less than 200nm,
In conjunction with table 2 using 3 kinds of difference D50 dispersion grinding aids obtain graphene slurry as a result, knowing that the partial size of dispersion grinding aid is small
It is a little more preferable.
According to table 2 as a result, embodiment 2 compares comparative example 2, addition dispersion grinding aid can be effectively reduced expanded graphite and shell
From when slurry viscosity, bonus point dissipates the partial size decline of grinding aid faster under identical milling time, and grinding efficiency is higher.Comparison
Example 3 the result shows that direct addition carbon black is not have that carbon black to be first crushed the effect that adds good.The result table of comparative example 4,5
Bright, addition dispersing agent PVP now commonly used in the trade can drastically reduce the viscosity of slurry, and efficiency, which is sanded, to be promoted, but slurry
Sedimentation stability is deteriorated.It is too many or very little that embodiment 5 and embodiment 6 show that the material for dispersing grinding aid cannot add, too much very little all
Pole piece resistivity is influenced to be deteriorated.Generally speaking, table 2 the result shows that addition dispersion grinding aid graphene comprehensive performance (such as:
Pole piece resistivity, sedimentation stability, grinding charge stripping efficiency) improve, and also viscosity is lower during the grinding process, phase under same time
It is higher than not adding the smaller viscosity that dispersion grinding aid obtains, it is higher to be crushed charge stripping efficiency.
According to fig. 2, it can be seen that carbon black broken particle can closely be attached in graphene surface, graphene sheet layer can be prevented
It returns and folds, be not necessarily to adhesive and organic dispersing agent.According to Fig. 3, it can be seen that carbon black is loosely adhered to stone in the form of a beading
The contact point of black alkene on piece, graphene and carbon black primary structure body and absorption point are all seldom, it is easy to fall off, and the addition of carbon black
It measures very high.
Although present disclosure is as above, present invention is not limited to this.Anyone skilled in the art are not departing from this
It in the spirit and scope of invention, can make various changes or modifications, therefore protection scope of the present invention should be with claim institute
Subject to the range of restriction.
Claims (10)
1. a kind of graphene slurry of the grinding aid containing dispersion, it is characterised in that, it is made of graphene, dispersion grinding aid and solvent；
Wherein, the dispersion grinding aid is carbon black particle, is less than by the partial size D50 of the carbon black particle of laser particle analyzer test
300nm。
2. it is according to claim 1 containing dispersion grinding aid graphene slurry, which is characterized in that the dispersion grinding aid by
The partial size D50 of the carbon black particle of laser particle analyzer test is less than 200nm.
3. the graphene slurry of the grinding aid according to claim 1 containing dispersion, which is characterized in that the dispersion grinding aid is
The broken body of carbon black primary structure body is made by the dispersion liquid of carbon black by high-pressure homogeneous crusher machine.
4. the graphene slurry of the grinding aid according to claim 1 containing dispersion, it is characterised in that, disperse grinding aid and graphite
Alkene mass ratio is 1:200~1:2.
5. the graphene slurry of the grinding aid according to claim 4 containing dispersion, it is characterised in that, disperse grinding aid and graphite
Alkene mass ratio is 1:100~1:7.
6. it is according to claim 1 containing dispersion grinding aid graphene slurry, which is characterized in that solvent be organic solvent,
The combination of any one or two kinds in resin.
7. the graphene slurry of the grinding aid according to claim 1 containing dispersion, which is characterized in that the graphene conductive slurry
The pole piece resistivity of material is 2.0~7.5 Ω cm.
8. a kind of preparation method of the graphene slurry of the grinding aid containing dispersion described in claim 1-7 any one, feature exist
In obtaining the dispersion liquid of carbon black first carbon black dispersion in solvent；The dispersion liquid of carbon black is carried out homogeneous with high pressure homogenizer
It is broken, obtain the dispersion liquid of the particle containing carbon black；Then the dispersion liquid of carbon black, expanded graphite and solvent are carried out with high speed disperser
Dispersion mixes, and obtains premix；Premix is finally put into progress liquid phase removing in sand mill, obtains the stone of the grinding aid containing dispersion
Black alkene slurry.
9. preparation method according to claim 8, which is characterized in that when liquid phase removes expanded graphite, sand mill linear speed
Degree is greater than 8m/s；The homogenization pressure of high pressure homogenizer is greater than 60MPa.
10. preparation method according to claim 8, which is characterized in that the expansion multiplying power of expanded graphite is more than or equal to 200
Times.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811606958.XA CN109455707A (en) | 2018-12-27 | 2018-12-27 | A kind of graphene slurry and preparation method thereof of the grinding aid containing dispersion |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811606958.XA CN109455707A (en) | 2018-12-27 | 2018-12-27 | A kind of graphene slurry and preparation method thereof of the grinding aid containing dispersion |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN109455707A true CN109455707A (en) | 2019-03-12 |
Family
ID=65615003
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201811606958.XA Pending CN109455707A (en) | 2018-12-27 | 2018-12-27 | A kind of graphene slurry and preparation method thereof of the grinding aid containing dispersion |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109455707A (en) |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110060818A (en) * | 2019-05-21 | 2019-07-26 | 郑州新世纪材料基因组工程研究院有限公司 | A kind of preparation method and application of low defect graphene conductive slurry |
| CN110620237A (en) * | 2019-10-25 | 2019-12-27 | 新奥石墨烯技术有限公司 | Conductive paste, preparation method and application thereof, and battery |
| CN111933949A (en) * | 2020-08-18 | 2020-11-13 | 东莞市海洲新材料科技有限公司 | Graphene conductive agent with adjustable sheet diameter distribution ratio, preparation method thereof, negative electrode and lithium ion battery |
| CN112573510A (en) * | 2020-12-30 | 2021-03-30 | 中国科学院过程工程研究所 | Graphene slurry and preparation method and application thereof |
| CN113122024A (en) * | 2021-03-29 | 2021-07-16 | 苏州大学 | Nano-sheet layered carbon black emulsion and preparation method and application thereof |
| CN113443620A (en) * | 2021-08-30 | 2021-09-28 | 湖南金阳烯碳新材料有限公司 | Preparation method and application of few-layer graphene powder |
| CN113640581A (en) * | 2021-08-10 | 2021-11-12 | 常州第六元素材料科技股份有限公司 | Graphene conductivity analysis method |
| CN113800505A (en) * | 2021-08-02 | 2021-12-17 | 江苏杉元科技有限公司 | Graphene aqueous slurry and preparation method thereof |
| CN114345480A (en) * | 2021-12-06 | 2022-04-15 | 山西沁新能源集团股份有限公司 | Wet grinding method for preparing graphite cathode material |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104464893A (en) * | 2014-12-26 | 2015-03-25 | 苏州格瑞丰纳米科技有限公司 | Small-blocking-agent-loaded graphene conductive slurry and preparation method and application thereof |
| CN105419095A (en) * | 2015-12-21 | 2016-03-23 | 赵社涛 | Method for producing carbon black composite powder material |
| CN106243836A (en) * | 2016-08-15 | 2016-12-21 | 青岛德通纳米技术有限公司 | A kind of graphene conductive carbon slurry and preparation method thereof |
| CN107492661A (en) * | 2017-08-17 | 2017-12-19 | 济宁利特纳米技术有限责任公司 | A kind of graphene lithium electricity electrocondution slurry and preparation method thereof |
| CN107628610A (en) * | 2017-10-30 | 2018-01-26 | 北京万源工业有限公司 | A kind of method that mechanical stripping method prepares graphene and graphene conductive liquid |
| CN108530996A (en) * | 2018-05-25 | 2018-09-14 | 北京航科航天科技有限公司 | A kind of one-step method prepares graphene-based water-soluble conducting ink and preparation method thereof |
| CN109652014A (en) * | 2018-12-26 | 2019-04-19 | 宁波杉元石墨烯科技有限公司 | A kind of graphene dispersion grinding aid and preparation method thereof |
-
2018
- 2018-12-27 CN CN201811606958.XA patent/CN109455707A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104464893A (en) * | 2014-12-26 | 2015-03-25 | 苏州格瑞丰纳米科技有限公司 | Small-blocking-agent-loaded graphene conductive slurry and preparation method and application thereof |
| CN105419095A (en) * | 2015-12-21 | 2016-03-23 | 赵社涛 | Method for producing carbon black composite powder material |
| CN106243836A (en) * | 2016-08-15 | 2016-12-21 | 青岛德通纳米技术有限公司 | A kind of graphene conductive carbon slurry and preparation method thereof |
| CN107492661A (en) * | 2017-08-17 | 2017-12-19 | 济宁利特纳米技术有限责任公司 | A kind of graphene lithium electricity electrocondution slurry and preparation method thereof |
| CN107628610A (en) * | 2017-10-30 | 2018-01-26 | 北京万源工业有限公司 | A kind of method that mechanical stripping method prepares graphene and graphene conductive liquid |
| CN108530996A (en) * | 2018-05-25 | 2018-09-14 | 北京航科航天科技有限公司 | A kind of one-step method prepares graphene-based water-soluble conducting ink and preparation method thereof |
| CN109652014A (en) * | 2018-12-26 | 2019-04-19 | 宁波杉元石墨烯科技有限公司 | A kind of graphene dispersion grinding aid and preparation method thereof |
Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110060818A (en) * | 2019-05-21 | 2019-07-26 | 郑州新世纪材料基因组工程研究院有限公司 | A kind of preparation method and application of low defect graphene conductive slurry |
| CN110620237A (en) * | 2019-10-25 | 2019-12-27 | 新奥石墨烯技术有限公司 | Conductive paste, preparation method and application thereof, and battery |
| CN111933949B (en) * | 2020-08-18 | 2022-04-05 | 东莞市海洲新材料科技有限公司 | Graphene conductive agent with adjustable sheet diameter distribution ratio, preparation method thereof, negative electrode and lithium ion battery |
| CN111933949A (en) * | 2020-08-18 | 2020-11-13 | 东莞市海洲新材料科技有限公司 | Graphene conductive agent with adjustable sheet diameter distribution ratio, preparation method thereof, negative electrode and lithium ion battery |
| CN112573510A (en) * | 2020-12-30 | 2021-03-30 | 中国科学院过程工程研究所 | Graphene slurry and preparation method and application thereof |
| CN113122024B (en) * | 2021-03-29 | 2022-04-15 | 苏州大学 | Nano-sheet layered carbon black emulsion and preparation method and application thereof |
| CN113122024A (en) * | 2021-03-29 | 2021-07-16 | 苏州大学 | Nano-sheet layered carbon black emulsion and preparation method and application thereof |
| CN113800505A (en) * | 2021-08-02 | 2021-12-17 | 江苏杉元科技有限公司 | Graphene aqueous slurry and preparation method thereof |
| CN113800505B (en) * | 2021-08-02 | 2023-07-25 | 江苏杉元科技有限公司 | Graphene aqueous slurry and preparation method thereof |
| CN113640581A (en) * | 2021-08-10 | 2021-11-12 | 常州第六元素材料科技股份有限公司 | Graphene conductivity analysis method |
| CN113640581B (en) * | 2021-08-10 | 2023-12-15 | 常州第六元素材料科技股份有限公司 | Graphene conductivity analysis method |
| CN113443620A (en) * | 2021-08-30 | 2021-09-28 | 湖南金阳烯碳新材料有限公司 | Preparation method and application of few-layer graphene powder |
| CN114345480A (en) * | 2021-12-06 | 2022-04-15 | 山西沁新能源集团股份有限公司 | Wet grinding method for preparing graphite cathode material |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN109455707A (en) | A kind of graphene slurry and preparation method thereof of the grinding aid containing dispersion | |
| CN106207094B (en) | A kind of lithium battery graphene conductive slurry and preparation method thereof | |
| CN107369823A (en) | A kind of lithium ion battery artificial composite cathode material of silicon/carbon/graphite and preparation method thereof | |
| KR101700355B1 (en) | Preparation method of carbon nanotube and dispersed composition of carbon nanotube | |
| CN103724869A (en) | Preparation method for mixture of polymer and graphene | |
| CN110350161B (en) | Preparation method of silicon-carbon negative electrode precursor | |
| CN104163417B (en) | A kind of method for peeling off preparing graphite alkene | |
| CN104916831A (en) | Preparation method of graphite silicon substrate composite cathode material | |
| WO2017036350A1 (en) | Lithium ion battery negative electrode material and preparation method thereof and lithium ion battery | |
| KR20150053693A (en) | Anode Materials of Lithium Ion Battery for Vehicle and Energy Storage, and Preparation Method thereof | |
| CN102181116B (en) | Carbon-nanotube-containing polymer nanocomposite and preparation method thereof | |
| CN106654269A (en) | Graphite negative electrode material used for power lithium ion battery and preparation method and application of graphite negative electrode material | |
| CN112331380A (en) | Composite conductive slurry and preparation method and application thereof | |
| CN112786855B (en) | Pomegranate-like structure silicon-carbon composite material, preparation method and application thereof | |
| CN111697225A (en) | Lithium iron phosphate anode slurry for lithium ion battery, preparation method of lithium iron phosphate anode slurry and anode plate | |
| CN110323416B (en) | Aqueous negative electrode stability slurry, preparation method thereof, negative electrode plate and lithium battery | |
| CN112186140B (en) | Silicon-based active composite conductive slurry applied to silicon-carbon cathode and cathode slurry mixing method | |
| CN104803408A (en) | Method for preparing modified nano-zinc oxide | |
| CN109652014A (en) | A kind of graphene dispersion grinding aid and preparation method thereof | |
| CN108039493A (en) | A kind of lithium ion battery electrocondution slurry and its preparation method and application | |
| CN103904303A (en) | Preparation method of high-capacity nanoscale lithium iron phosphate electrode plate with long service life | |
| CN109509869A (en) | A kind of lithium ion cell positive dry mixing technique | |
| CN107706399B (en) | One-dimensional carbon fiber/carbon nanotube composite material, preparation method and application thereof | |
| CN1884056A (en) | Carbon material and nano silicon composite materials and method for preparing same and use thereof | |
| CN103137946B (en) | A kind of anthraquinone lithium battery positive pole and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| CB02 | Change of applicant information |
Address after: 213102 No. 666, Daluo Road, Yaoguan Town, Changzhou Economic Development Zone, Jiangsu Province Applicant after: Jiangsu Shanyuan Technology Co., Ltd Address before: 315000 No. 238, Yunlin Middle Road, Wangchun Industrial Park, Haishu District, Ningbo, Zhejiang Applicant before: Ningbo Shanyuan graphene Technology Co., Ltd |
|
| CB02 | Change of applicant information | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20190312 |
|
| WD01 | Invention patent application deemed withdrawn after publication |