CN107161993B - High concentration graphene slurry and preparation method thereof and device - Google Patents
High concentration graphene slurry and preparation method thereof and device Download PDFInfo
- Publication number
- CN107161993B CN107161993B CN201710536333.XA CN201710536333A CN107161993B CN 107161993 B CN107161993 B CN 107161993B CN 201710536333 A CN201710536333 A CN 201710536333A CN 107161993 B CN107161993 B CN 107161993B
- Authority
- CN
- China
- Prior art keywords
- graphene
- graphene slurry
- expanded graphite
- preparation
- dispersing agent
- 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.)
- Active
Links
Landscapes
- Carbon And Carbon Compounds (AREA)
Abstract
The present invention provides a kind of high concentration graphene slurry and preparation method thereof and devices.The present invention is by the way that expanded graphite and dispersing agent to be added portionwise, the graphene slurry of high concentration has been prepared without being concentrated in the method that solvent once is added.The present invention provides the preparation facilities of slurry, make the further mechanization of the preparation process of graphene slurry, are more advantageous to the large-scale production of high concentration graphene slurry.
Description
Technical field
The present invention relates to field of graphene, fill more particularly to a kind of high concentration graphene slurry, preparation method and preparation
It sets.
Background technique
Graphene is attracting more and more research teams to carry out it due to the performances such as its excellent mechanics, conduction, thermally conductive
Theoretical and application study.Graphene price is higher, and exploitation green, high-quality, extensive, high concentration preparation process become current stone
Can the research hotspot and graphene in black alkene field realize industrial application, realize the key of the update of traditional product
One.
Liquid phase removing expanded graphite prepare graphene be realize graphene green, high-quality, the method for prepare with scale it
One.Expanded graphite is non-polar material, have excellent adsorptivity, high 10 times of oil factor specific activity charcoal or more, to polar water
Adsorb poor, but Surfactant adsorption from aqueous solution value is high.Preparing aqueous, oiliness (NMP phase, DMF solvent) graphene
In slurry process, due to the high adsorption solvent performance of expanded graphite, expanded graphite, surfactant, solvent mixture are difficult
Continuous suspension is formed, high concentration graphite slurry is especially prepared, initial feed shows as mortar shape after mixing, leads to ultrasonic wave
It can not be propagated in solvent medium, will not more enter expanded graphite interlayer and form " cavitation ", to cause removing expansion stone
Black efficiency reduces or failure.
It is larger to oil-based solvent and aqueous surfactant solution adsorbance due to the excellent adsorptivity of expanded graphite, tradition
Preparing high concentration graphene slurry is the method using concentrating low-concentration graphene slurry.Being separated by filtration concentration will increase preparation work
Sequence, since graphene film diameter is small, it is desirable that filter cloth aperture is smaller, then energy consumption is higher, and there are also inevitable evaporating, emitting, dripping or leaking of liquid or gas, generates big
Measure filtrate sewage, and cleaning filter cloth sewage.Evaporation and concentration will increase preparation section, and energy consumption is higher, while a large amount of evaporation water needs
Configuration evaporation water collection system, increases cost.
Summary of the invention
It is a primary object of the present invention to provide a kind of high concentration graphene slurry and preparation method thereof and device,
The technical issues of solution, is to provide the preparation method and preparation facilities of a kind of simpler high concentration graphene slurry, from
And it is more suitable for practical.
The object of the invention to solve the technical problems adopts the following technical solutions to realize.
A kind of preparation method of graphene slurry proposed according to the present invention, including, weigh expanded graphite, dispersing agent and molten
The expanded graphite is divided into N parts by agent, respectively first part of expanded graphite ..., N parts of expanded graphites, the N
For natural number, and the N is greater than or equal to 2, the dispersing agent is divided into M part, respectively first part is dispersed
Agent ..., M parts of dispersing agents, the M be natural number, the M be greater than or equal to 2；By first part of expansion stone
Ink, first part of dispersing agent and whole solvents carry out the first stirring, and the first mixed liquor is obtained after stirring；By first mixed liquor
It is placed in ultrasonic system, after ultrasound, obtains graphene slurry presoma；Remaining expanded graphite and dispersing agent are stirred in batches, and are divided
It criticizes and is added in the ultrasonic system, after ultrasound, obtain the graphene slurry, it is described in terms of mass percentage
The concentration of graphene is greater than or equal to 3% in graphene slurry.
The object of the invention to solve the technical problems also can be used following technical measures and further realize.
Preferably, the preparation method of a kind of graphene slurry above-mentioned, wherein the expanded graphite and the dispersion
The mass ratio of agent is 1: 0.1-1；The mass ratio of the expanded graphite and the solvent is 30-3: 100.
Preferably, the preparation method of a kind of graphene slurry above-mentioned, wherein the dispersing agent includes alkyl phenol and ring
Oxidative ethane condensation product, alkyl phenol polyoxyethylene ether, fatty alcohol and ethylene oxide condensate, castor oil and ethylene oxide condensate,
One or two or more kinds of combinations of polyvinylpyrrolidone, block polyether.
Preferably, the preparation method of a kind of graphene slurry above-mentioned, wherein the solvent includes water, NMP (N- methyl
Pyrrolidones) or DMF (n,N-Dimethylformamide).
Preferably, the preparation method of a kind of graphene slurry above-mentioned, wherein the expanded graphite be divided into first part it is swollen
Swollen graphite, second part of expanded graphite ..., N parts of expanded graphites, the N is greater than or equal to 3, the dispersing agent point
For first part of dispersing agent, second part of dispersing agent ..., M parts of dispersing agents, the M be greater than or equal to 3；By described
Two parts of expanded graphites and second part of dispersing agent carry out the second stirring, and the second mixed liquor is obtained after stirring；By described
Two mixed liquors are placed in ultrasonic system, after ultrasound, obtain graphene slurry intermediate；In terms of mass percentage, the graphite
The concentration of graphene and the difference of the concentration of graphene in the graphene slurry presoma are less than in alkene slurry intermediate
3%.
Also the following technical solution is employed for the object of the invention to solve the technical problems to realize.
A kind of graphene slurry proposed according to the present invention, the graphene slurry is by described in any item systems above-mentioned
Preparation Method is prepared.
The object of the invention to solve the technical problems also can be used following technical measures and further realize.
Preferably, a kind of graphene slurry above-mentioned, wherein the concentration of graphene is 3%- in the graphene slurry
25%, percentage herein is mass percent.
Preferably, a kind of graphene slurry above-mentioned, wherein the D50 of graphene partial size is less than in the graphene slurry
10um, D90 are less than 30um.
Also the following technical solution is employed for the object of the invention to solve the technical problems to realize.
The preparation facilities of a kind of graphene slurry proposed according to the present invention, according to described in any item preparation sides above-mentioned
Method, the preparation facilities include ultrasonic system, stirring system and the circulatory system, wherein the ultrasonic system is used for institute
The expanded graphite stated, dispersing agent and solvent carry out ultrasound, the stirring system be used for by the expanded graphite, dispersing agent,
Solvent is stirred, and the circulatory system is used to for the material in the stirring system being added in the ultrasonic system,
Alternatively, the material in the ultrasonic system is recycled.
The object of the invention to solve the technical problems also can be used following technical measures and further realize.
Preferably, the preparation facilities of a kind of graphene slurry above-mentioned, wherein the stirring system includes mechanical stirring
Device, magnetic stirring apparatus or distributing ultrasonic stirrer.
Preferably, the preparation facilities of a kind of graphene slurry above-mentioned, wherein the ultrasonic system includes cooling device.
Preferably, the preparation facilities of a kind of graphene slurry above-mentioned, wherein the stirring system includes the first connection
End and second connection end, first connecting pin and second connection end are connect with the ultrasonic system respectively, form first
Connecting path and the second connecting path, the circulatory system are located at second connecting path.
Preferably, the preparation facilities of a kind of graphene slurry above-mentioned, wherein first connecting path includes first
Switch, second connecting path include second switch, and the preparation facilities also includes third connecting path, and described the
Comprising third switch and the 4th switch in three connecting paths, it is logical that the third connecting path is separately connected first connection
Road and the second connecting path, form circulation path, and the first switch, second switch, third switch, the 4th switch are respectively positioned on
The circulation path.
By above-mentioned technical proposal, high concentration graphene slurry provided by the invention and preparation method thereof and device, at least
It has the advantage that
1, the present invention provides a kind of preparation methods of high concentration graphene slurry.
The preparation method of high concentration graphene slurry provided by the invention, mainly comprises the steps that
Firstly, preparing the graphene mother liquor of low concentration.Demi-inflation graphite, part dispersing agent and whole solvents are being stirred
It mixes in system and is pre-mixed, and mixed material is put into and carries out ultrasound in ultrasonic system.At this point, due to expanded graphite
Additional amount is less, and the ultrasonic wave that ultrasonic system generates can stablize propagation in solvent medium, makes the removing of expanded graphite more
Quickly, uniformly；Also, solvent once is added to release system, is conducive to ultrasonic wave fast propagation in solvent medium, into one
Step improves the peeling rate of expanded graphite；The quick, stable of ultrasonic wave is propagated, and makes the graphene obtained after removing in a solvent
Quickly diffusion, it is not easy to reunite, further improve the stability of graphene slurry.
Secondly, due to micron order in mother liquor and being received during low concentration graphene slurry is further carried out enrichment
Meter level graphene enters the micropore, macropore and super large duct of expanded graphite, and the graphene edge of cleat shape squeezes into expanded graphite
Interlayer can further increase the interlamellar spacing of expanded graphite.Meanwhile isolated graphene can be used as carrier, wrap up its carrying
Dispersing agent enter the interlayer of expanded graphite, cause dispersing agent to enter expanded graphite interlayer, improve nonpolar expanded graphite and
The wetting action of solvent provides the channel that ultrasonic wave enters expanded graphite interlayer by solvent medium, improves ultrasonic removing
Effect reduces ultrasonic splitting time.
2, the present invention provides a kind of preparation method of high concentration graphene slurry, the rows of the pollutants such as this method free from admixture
It puts, the slurry being prepared is not necessarily to subsequent processing, can be used directly.
In the graphene slurry that preparation method provided by the invention is prepared, the mass percentage of graphene is 3-
25%, belong to high concentration graphene slurry.In the prior art, the method for preparing high concentration graphene slurry is by low concentration graphite
Alkene slurry is concentrated, and concentration process has energy consumption height, easily causes the defects of environmental pollution.High concentration graphite provided by the invention
The preparation method of alkene slurry is not required to concentration step, therefore, without the discharge of any pollutant, and the graphene slurry being prepared
Material is more stable, not easy to reunite.
3, the present invention provides a kind of preparation facilities of high concentration graphene slurry, preparation process is simple, is more conducive to
Large-scale production.
The preparation facilities of high concentration graphene slurry provided by the invention, can successional progress high concentration graphene slurry
Preparation, improve high concentration graphene slurry preparation mechanization；And without carrying out " concentration " process, reduce preparation step
Suddenly, preparation process is simplified, the large-scale production of high concentration graphene slurry is more conducive to.
The above description is only an overview of the technical scheme of the present invention, in order to better understand the technical means of the present invention,
And can be implemented in accordance with the contents of the specification, the following is a detailed description of the preferred embodiments of the present invention and the accompanying drawings.
Detailed description of the invention
Fig. 1 is the preparation facilities of high concentration graphene slurry provided in an embodiment of the present invention.
The flange of 11 Vltrasonic devices, the flange of 12 Vltrasonic devices, 13 water-cooling wall water outlets, 14 energy-collecting ultrasonic sticks, 15 water coolings
Wall, 16 ultrasonic system reaction kettle cavitys, 17 water-cooling wall water inlets；
21 stirring systems；
31 peristaltic pumps, 32 Wriggling Pump Heads, 33 size circulations directions, 34 first switches, 35 second switches, 36 thirds switch,
37 the 4th switches.
Specific embodiment
It is of the invention to reach the technical means and efficacy that predetermined goal of the invention is taken further to illustrate, below in conjunction with
Attached drawing and preferred embodiment, it is specific to high concentration graphene slurry proposed according to the present invention and preparation method thereof and device
Embodiment, structure, feature and its effect, detailed description is as follows.In the following description, different " embodiment " or " implementation
What example " referred to is not necessarily the same embodiment.In addition, the special characteristic, structure or feature in one or more embodiments can be by any
Suitable form combination.
The present invention provides a kind of preparation methods of graphene slurry.
The preparation method of graphene slurry provided by the invention includes weighing expanded graphite, dispersing agent and solvent, will be described
Expanded graphite be divided into N parts, respectively the first expanded graphite ..., N expanded graphite, the N is greater than or equal to 2, will
The dispersing agent is divided into M parts, respectively the first dispersing agent ..., M dispersing agent, the M is greater than or equal to 2；By institute
The first expanded graphite, the first dispersing agent and the whole solvents stated carry out the first stirring, and the first mixed liquor is obtained after stirring；It will be described
The first mixed liquor be placed in ultrasonic system, ultrasound after, obtain graphene slurry presoma；Stir in batches remaining expanded graphite and
Dispersing agent, and be added portionwise in the ultrasonic system, after ultrasound, the graphene slurry is obtained, is contained with quality percentage
Meter, the concentration of graphene is greater than or equal to 3% in the graphene slurry.
The present invention provides a kind of preparation methods of high concentration graphene slurry.Required material includes expanded graphite, divides
Expanded graphite therein and dispersing agent are added portionwise for powder and solvent, and solvent once therein is added.It needs to illustrate
It is that M and N herein can be equal, it can also be unequal.The weight of every part of expanded graphite can be identical, can not also be identical；Often
The weight of part dispersing agent can be identical, can not also be identical.
" stirring remaining expanded graphite and dispersing agent in batches " herein can explain are as follows: if being by remaining expanded graphite
Second part of expanded graphite, third part expanded graphite, remaining dispersing agent is second part of dispersing agent, third part dispersing agent, then by the
Two parts of expanded graphites and second part of dispersing agent are stirred, and obtain the second mixed liquor, by third part expanded graphite and third part point
Powder is stirred, and obtains third mixed liquor.
" being added portionwise in the ultrasonic system " herein can explain are as follows: second obtained will stir in batches after mixes
It closes liquid and third mixed liquor is added separately in ultrasonic system.
Further, the mass ratio of the expanded graphite and the dispersing agent is 1: 0.1-1；The expansion stone
The black mass ratio with the solvent is 30-3: 100.
The present invention further defines the mass ratio of expanded graphite, dispersing agent and solvent.According to required graphene slurry
Quality and graphene slurry in graphene mass percentage, calculate expanded graphite and solvent dosage.It needs to illustrate
It is that the used in amounts strict control of dispersing agent influences the effect of graphene slurry if the dosage of dispersing agent is excessive in the present invention
Performance, while graphene slurry electric conductivity is greatly reduced, if the dosage of dispersing agent is very few, the wetting of graphite is insufficient,
Ultrasonic peeling effect is seriously affected, peeling rate is slow, while the graphene slurry being prepared easily is reunited.
Further, the dispersing agent includes condensation compound of alkyl phenol and epoxy ethane, alkyl phenol polyoxyethylene ether, fat
Alcohol and one of ethylene oxide condensate, castor oil and ethylene oxide condensate, polyvinylpyrrolidone, block polyether or two
Kind or more combination.
Further, the expanded graphite be divided into the first expanded graphite, the second expanded graphite ..., N expansion stone
Ink, the N be greater than or equal to 3, the dispersing agent be divided into the first dispersing agent, the second dispersing agent ..., M dispersing agent,
The M is greater than or equal to 3；Second expanded graphite and second dispersing agent are subjected to the second stirring, after stirring
Obtain the second mixed liquor；Second mixed liquor is placed in ultrasonic system, after ultrasound, obtains graphene slurry intermediate；With
Mass percentage agent, in the graphene slurry intermediate in the concentration of graphene and the graphene slurry presoma
The difference of the concentration of graphene is less than 3%.
The present invention further defines the concentration difference of adjacent two graphenes slurry.The restriction of this concentration difference, on the one hand in order to
The preparation efficiency of graphene slurry is improved, on the other hand in order to improve the stability of graphene slurry.The study found that if adding every time
The amount of the expanded graphite entered is larger, then is unfavorable for the diffusion of the graphene obtained after removing, Yi Fasheng agglomeration, at this point, needing
Twice ultrasonic is carried out, or even ultrasonic three times, to improve the dispersion stabilization of graphene in the slurry.As it can be seen that ultrasonic time is not
It is directly proportional to the dosage of expanded graphite.The concentration difference that the present invention limits is conducive to the graphene that removing obtains and quickly spreads, improves
Preparation efficiency.On the other hand, the graphene slurry removed quickly is spread in a solvent, keeps graphene primary in a solvent
Property " occupy-place ", " positioning ", be not necessarily to secondary diffusion, improve the dispersibility of graphene, and then improve the stabilization of graphene slurry
Property.
Invention further provides a kind of graphene slurries.
Using the preparation method of graphene slurry provided by the invention, the graphite that mass concentration is 3-25% has been prepared
Alkene slurry, and the D50 of graphene partial size is less than 10um in slurry, D90 is less than 30um (partial size is measured by laser particle analyzer).
Invention further provides a kind of preparation facilities of graphene slurry.
Device provided by the invention includes ultrasonic system, stirring system and the circulatory system.
The ultrasonic system is used for the removing of expanded graphite, and the stirring system is used for the stirring of material, including will
Expanded graphite, dispersing agent and solvent are stirred, alternatively, expanded graphite and dispersing agent are stirred.The circulatory system
It is added in ultrasonic system for the material after stirring, alternatively, the material in the ultrasonic system is recycled.
Firstly, the material of stirring system is added slowly in ultrasonic system by the circulatory system, the addition of material is limited
Amount, the ultrasonic wave for being conducive to ultrasonic system generation are propagated in a solvent, improve charge stripping efficiency.
Secondly, the circulatory system recycles the material in ultrasonic system.Expanded graphite is in ultrasonic reaction system, through super
The graphene that sound is stripped out is not easy to spread in a solvent, is especially diffused in the graphene slurry of high concentration.This hair
The preparation facilities of bright offer will have the size circulations of graphene using the circulatory system, so that slurry is in flow regime, play
The effect futher stirred, the combination for increasing graphene and solvent and the stability after combination.In addition, circulator also rises
Arrived the effect of temporary storing graphite alkene slurry, the graphene that will be separated, by the circulatory system, reduce graphene with it is swollen
(because since polarity is similar, isolated graphene and expanded graphite are easy to happen reunion in solvent for the reunion of swollen graphite
Phenomenon).
Again, the circulatory system makes isolated graphene be kept in motion, and has been further driven to have cleat shape
Graphene edge squeeze into expanded graphite interlayer, further improve the charge stripping efficiency of expanded graphite.
Further, the circulatory system is peristaltic pump, and the circulating fluid volume of peristaltic pump is less than 30kg/ minutes.
Embodiment 1
Prepare the aqueous slurry 10kg that graphene slurry concentration is 10wt%.Dispersing agent is polyvinylpyrrolidone, poly- second
Alkene pyrrolidone and expanded graphite mass ratio 0.3.Expanded graphite needed for calculating slurry is 1kg, dispersing agent 0.3kg and solvent
Gross mass is 8.7kg.
The preparation facilities of graphene slurry provided in this embodiment is as shown in Figure 1.In device provided in this embodiment, ultrasound
System includes the flange 11 of Vltrasonic device, the flange 12 of Vltrasonic device, water-cooling wall water outlet 13, energy-collecting ultrasonic stick 14, water-cooling wall
15, ultrasonic system reaction kettle cavity 16, water-cooling wall water inlet 17；Peristaltic pump 31 includes Wriggling Pump Head 32.At this point, first switch
34, second switch 35, third switch 36, the 4th switch 37 is in closed state.
The ultrasonic vibration stick that the ultrasonic system that the present embodiment uses produces for Handan beauty along Mechanical Equipment Company, power 3kW,
Frequency 20kHz, ultrasonic vibration stick cross-sectional diameter 50mm.Peristaltic pump is that Lei Fu Liquidia Technologies Inc. in Baoding produces speed-regulating type wriggling
Pump, range of flow 1.8-6000 ml/min, the range of speeds: 30-600RPM, pump head port number 1, hose diameter 36mm, single-pass
80~6000 ml/min of road flow.Stirring system is magnetic agitation.
The preparation facilities of graphene slurry provided in this embodiment, single set can prepare thousand grams/times of 0.3-40.
Step 1: by 0.3kg expanded graphite and 0.09kg polyvinylpyrrolidone, 8.7kg water in stirring system 21 into
Row stirring (stirring system in the present embodiment is magnetic stirring apparatus), after mixing evenly, opens first switch 34 and second switch
35, that is, the first connecting path and the second connecting path (circulator is located at the second connecting path) are got through, using peristaltic pump
31 are slowly positioned at the material in stirring system in ultrasonic system.Method are as follows: open the water inlet of the water-cooling wall 15 of ultrasonic system
17 and water outlet 13, so that cooling water is in recurrent state, opens peristaltic pump 31 according to direction described in Fig. 1, peristaltic pump follows
Ring liquid measure 10kg/ minutes, ultrasonic reaction system is opened, the material in stirring system is made to fully enter the reaction kettle chamber of ultrasonic system
In body 16；
Step 2: opening third switch 36 and the 4th switch 37, closes first switch 34 and second switch 35, ultrasound removing
To D50 < 5um, D90 < 15um, graphene slurry mother liquor is obtained；
Step 3: 0.3kg expanded graphite and 0.09kg polyvinylpyrrolidone are added in stirring system 21 go forward side by side again
Row stirring after the completion of stirring, opens first switch 34 and second switch 35, closes third switch 36 and the 4th switch 37, and adopt
The material in stirring system is fully entered in reaction kettle cavity 16 with peristaltic pump 31；
Step 4: opening third switch 36 and the 4th switch 37, closes first switch 34 and second switch 35, ultrasound removing
To D50 < 5um, D90 < 15um, enrichment graphene slurry is obtained；
Repeat the above steps three and step 4, obtains the watersoluble plumbago alkene slurry that 10kg graphene concentration is 10wt%.
The number of plies of graphene is to have within standing 1 month or more less than 10 layers in the graphene slurry that the present embodiment is prepared
It is slight to reunite, and the graphene film reunited is stirred energetically or ultrasonic power, the graphene film of reunion are disconnected from each other.
The preparation time of the present embodiment high concentration aqueous's graphene slurry is about less than 5 hours, in the prior art, if obtaining phase
With the graphene slurry of concentration, after through centrifugal concentrating or filtering concentration, liquid relief, redisperse into uniform sizing material, used time 20
Hour or more, while evaporating, emitting, dripping or leaking of liquid or gas is severe in concentration process, process is more, and sewage quantity is big.
Similar, using the combination of other dispersing agents provided by the invention and different dispersing agents, can also be prepared
The watersoluble plumbago alkene slurry of 10wt%.The dosage of expanded graphite and dispersing agent is further increased, can be prepared 25wt%'s
Watersoluble plumbago alkene slurry.
Embodiment 2
Prepare the NMP phase slurry 20kg that graphene slurry concentration is 5wt%.Dispersing agent is total for polyoxypropylene polyoxyethylene
Polymers, dispersing agent and expanded graphite mass ratio 0.2.Expanded graphite needed for calculating slurry is 1kg, dispersing agent 0.2kg and solvent
Gross mass is 18.8kg.
Step 1: 0.25kg expanded graphite and 0.05kg polyoxypropylene polyoxyethylene copolymer, 18.8kg water are being stirred
It is stirred, the material in stirring system is slowly positioned in ultrasonic system using peristaltic pump 31, peristaltic pump follows in system 21
Ring liquid measure 15kg/ minutes, ultrasonic reaction system is opened, the material in stirring system is made to fully enter the reaction kettle chamber of ultrasonic system
In body 16；
Step 2: opening third switch 36 and the 4th switch 37, closes first switch 34 and second switch 35, ultrasound removing
To D50 < 3um, D90 < 10um, graphene slurry mother liquor is obtained；
Step 3: stirring system is added in 0.25kg expanded graphite and 0.05kg polyoxypropylene polyoxyethylene copolymer again
It in system 21 and is stirred, after the completion of stirring, opens first switch 34 and second switch 35, close third switch 36 and the 4th and open
37 are closed, and is fully entered the material in stirring system in reaction kettle cavity 16 using peristaltic pump 31；
Step 4: opening third switch 36 and the 4th switch 37, closes first switch 34 and second switch 35, ultrasound removing
To D50 < 3um, D90 < 10um, enrichment graphene slurry is obtained；
Repeat the above steps three and step 4, obtains the NMP phase graphene slurry that 20kg graphene concentration is 5wt%.
Other preparation process are same as Example 1 or similar.
The number of plies of graphene is to have within standing 1 month or more less than 10 layers in the graphene slurry that the present embodiment is prepared
It is slight to reunite, and the graphene film reunited is stirred energetically or ultrasonic power, the graphene film of reunion are disconnected from each other.
The preparation time of the present embodiment high concentration NMP phase graphene slurry is about less than 5 hours, in the prior art, if obtaining
The graphene slurry of same concentrations, after through centrifugal concentrating or filtering concentration, liquid relief, redisperse into uniform sizing material, the used time
20 hours or more, while evaporating, emitting, dripping or leaking of liquid or gas is severe in concentration process, process is more, and sewage quantity is big.
Similar, using the combination of other dispersing agents provided by the invention and different dispersing agents, can also be prepared
The NMP phase graphene slurry of 5wt%.The dosage of expanded graphite and dispersing agent is further increased, can be prepared 25wt%'s
NMP phase graphene slurry.
Using the method similar with embodiment 2, the DMP phase graphene slurry of 3-25wt% can be prepared.
In the above-described embodiments, it all emphasizes particularly on different fields to the description of each embodiment, there is no the portion being described in detail in some embodiment
Point, reference can be made to the related descriptions of other embodiments.
It is understood that the correlated characteristic in above-mentioned apparatus can be referred to mutually.In addition, in above-described embodiment " the
One ", " second " etc. is and not represent the superiority and inferiority of each embodiment for distinguishing each embodiment.
In the instructions provided here, numerous specific details are set forth.It is to be appreciated, however, that implementation of the invention
Example can be practiced without these specific details.In some instances, well known structure and skill is not been shown in detail
Art, so as not to obscure the understanding of this specification.
Similarly, it should be understood that in order to simplify the disclosure and help to understand one or more of the various inventive aspects, In
Above in the description of exemplary embodiment of the present invention, each feature of the invention is grouped together into single implementation sometimes
In example, figure or descriptions thereof.However, the device of the disclosure should not be construed to reflect an intention that i.e. required guarantor
Shield the present invention claims features more more than feature expressly recited in each claim.More precisely, as following
Claims reflect as, inventive aspect is all features less than single embodiment disclosed above.Therefore,
Thus the claims for following specific embodiment are expressly incorporated in the specific embodiment, wherein each claim itself
All as a separate embodiment of the present invention.
Those skilled in the art will understand that can be carried out adaptively to the component in the device in embodiment
Change and they are arranged in one or more devices unlike this embodiment.It can be the component combination in embodiment
At a component, and furthermore, they can be divided into multiple subassemblies.In addition at least some of such feature is mutual
It, can be using any combination to institute disclosed in this specification (including adjoint claim, abstract and attached drawing) except repulsion
There are feature and all components of so disclosed any device to be combined.Unless expressly stated otherwise, this specification (including
Adjoint the claims, abstract and drawings) disclosed in each feature can be by providing the substitution of identical, equivalent, or similar purpose
Feature replaces.
In addition, it will be appreciated by those of skill in the art that although some embodiments described herein include other embodiments
In included certain features rather than other feature, but the combination of the feature of different embodiments mean it is of the invention
Within the scope of and form different embodiments.For example, in the following claims, embodiment claimed is appointed
Meaning one of can in any combination mode come using.Various component embodiments of the invention can be implemented in hardware, or
It is implemented in a combination thereof.
It should be noted that the above-mentioned embodiments illustrate rather than limit the invention, and ability
Field technique personnel can be designed alternative embodiment without departing from the scope of the appended claims.In the claims,
Any reference symbol between parentheses should not be configured to limitations on claims.Word "comprising" does not exclude the presence of not
Component or component listed in the claims.Word "a" or "an" before component or component does not exclude the presence of multiple
Such component or component.The present invention can be realized by means of including the device of several different components.It is several listing
In the claim of component, several in these components, which can be through the same component item, to be embodied.Word first,
Second and the use of third etc. do not indicate any sequence.These words can be construed to title.
Heretofore described numberical range includes numerical value all within the scope of this, and including any two within the scope of this
The value range of numerical value composition.For example, " concentration of graphene is 3%-25% in the graphene slurry ", this numberical range packet
Include numerical value all between " 3-25 ", and including any two numerical value within the scope of this (such as: 10, the 20) value range formed
(10-20)；The different numerical value of the same index occurred in all embodiments of the invention, can in any combination, compositing range value.
Technical characteristic in the claims in the present invention and/or specification can be combined, and a combination thereof mode is not limited to weigh
The combination obtained in benefit requirement by adduction relationship.It is combined by the technical characteristic in claim and/or specification
The technical solution and protection scope of the present invention arrived.
The above described is only a preferred embodiment of the present invention, be not intended to limit the present invention in any form, according to
According to technical spirit any simple modification, equivalent change and modification to the above embodiments of the invention, this hair is still fallen within
In the range of bright technical solution.
Claims (10)
1. a kind of preparation method of graphene slurry, it is characterised in that: including,
Expanded graphite, dispersing agent and solvent are weighed, the expanded graphite is divided into N parts, the N is natural number, and described
N be greater than or equal to 2, the dispersing agent is divided into M part, the M is natural number, and the M is more than or equal to 2；
First part of expanded graphite, first part of dispersing agent and whole solvents are subjected to the first stirring, the first mixed liquor is obtained after stirring；
First mixed liquor is placed in ultrasonic system, after ultrasound, obtains graphene slurry presoma；
Remaining expanded graphite and dispersing agent are stirred in batches, and is added portionwise in the ultrasonic system, after ultrasound, obtain stone
Black alkene slurry,
In terms of mass percentage, the concentration of graphene is greater than or equal to 3% in the graphene slurry.
2. a kind of preparation method of graphene slurry according to claim 1, it is characterised in that:
The mass ratio of the expanded graphite and the dispersing agent is 1:0.1-1；
The mass ratio of the expanded graphite and the solvent is 30-3:100.
3. a kind of preparation method of graphene slurry according to claim 1, it is characterised in that:
The dispersing agent includes condensation compound of alkyl phenol and epoxy ethane, alkyl phenol polyoxyethylene ether, fatty alcohol and ethylene oxide
The group of one of condensation product, castor oil and ethylene oxide condensate, polyvinylpyrrolidone, block polyether or two kinds or more
It closes.
4. a kind of preparation method of graphene slurry according to claim 1, it is characterised in that:
The solvent includes water, NMP or DMF.
5. a kind of preparation method of graphene slurry according to claim 1, it is characterised in that:
The expanded graphite is divided into N parts, and the N is greater than or equal to 3, and the dispersing agent is divided into M parts, and the M is greater than
Or it is equal to 3；
Second part of expanded graphite and second part of dispersing agent are subjected to the second stirring, the second mixed liquor is obtained after stirring；
Second mixed liquor is placed in ultrasonic system, after ultrasound, obtains graphene slurry intermediate；
In terms of mass percentage, in the graphene slurry intermediate before the concentration of graphene and the graphene slurry
The difference of the concentration of graphene in body is driven less than 3%.
6. a kind of graphene slurry, it is characterised in that:
The graphene slurry is prepared by preparation method of any of claims 1-5；
In terms of mass percentage, the concentration of graphene is 3%-10% in the graphene slurry；
The D50 of graphene partial size is less than 10um in the graphene slurry, and D90 is less than 30um.
7. a kind of preparation facilities of graphene slurry, it is characterised in that:
Preparation method according to any one of claims 1-5, the preparation facilities include ultrasonic system, stirring system
And the circulatory system,
Wherein, the ultrasonic system is used to carrying out the expanded graphite, dispersing agent and solvent into ultrasound, the stirring system
For the expanded graphite, dispersing agent, solvent to be stirred, the circulatory system is used for the stirring system system
In material be added in the ultrasonic system, alternatively, the material in the ultrasonic system is recycled；The stirring
System includes the first connecting pin and second connection end, and first connecting pin and second connection end are with the ultrasound respectively
System connection is respectively formed the first connecting path and the second connecting path, and it is logical that the circulatory system is located at second connection
Road.
8. a kind of preparation facilities of graphene slurry according to claim 7, it is characterised in that:
The stirring system includes mechanical agitator, magnetic stirring apparatus or distributing ultrasonic stirrer.
9. a kind of preparation facilities of graphene slurry according to claim 7, it is characterised in that:
The ultrasonic system includes cooling device.
10. a kind of preparation facilities of graphene slurry according to claim 7, it is characterised in that:
First connecting path includes first switch, and second connecting path includes second switch,
The preparation facilities also includes third connecting path, is opened in the third connecting path comprising third switch and the 4th
It closes,
The third connecting path is separately connected first connecting path and the second connecting path, forms circulation path,
The first switch, second switch, third switch, the 4th switch are respectively positioned on the circulation path.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710536333.XA CN107161993B (en) | 2017-07-03 | 2017-07-03 | High concentration graphene slurry and preparation method thereof and device |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710536333.XA CN107161993B (en) | 2017-07-03 | 2017-07-03 | High concentration graphene slurry and preparation method thereof and device |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN107161993A CN107161993A (en) | 2017-09-15 |
| CN107161993B true CN107161993B (en) | 2019-11-12 |
Family
ID=59822542
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710536333.XA Active CN107161993B (en) | 2017-07-03 | 2017-07-03 | High concentration graphene slurry and preparation method thereof and device |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107161993B (en) |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108012349A (en) * | 2017-11-28 | 2018-05-08 | 扬州地脉远红地暖科技有限公司 | A kind of graphene carbon fibre with high-efficiency energy-saving ground heating line with heating function and its manufacturing process |
| CN109467658A (en) * | 2018-11-13 | 2019-03-15 | 大同新成新材料股份有限公司 | A kind of preparation method and preparation facilities of modified graphene slurry |
| CN111392720B (en) * | 2020-03-23 | 2022-04-26 | 北京石墨烯研究院 | High-concentration graphene oxide solution and preparation method and application thereof |
| CN113731330A (en) * | 2021-09-07 | 2021-12-03 | 中国人民解放军陆军装甲兵学院 | Device of high efficiency preparation graphite alkene magnetic powder |
Family Cites Families (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2013172350A1 (en) * | 2012-05-14 | 2013-11-21 | 国立大学法人 東京大学 | Novel graphene nanodispersion and method for preparing same |
| CN104772064B (en) * | 2015-03-31 | 2017-01-18 | 山东玉皇新能源科技有限公司 | Method for preparing grapheme dispersion liquid |
| CN104860290A (en) * | 2015-04-22 | 2015-08-26 | 湖南元素密码石墨烯研究院（有限合伙） | Apparatus for preparing fluorinated graphene |
| CN104979563B (en) * | 2015-07-19 | 2017-03-08 | 厦门凯纳石墨烯技术股份有限公司 | The preparation method of nitridation Graphene lithium-ion-power cell slurry |
| CN105692605B (en) * | 2016-04-05 | 2017-12-22 | 江苏省特种设备安全监督检验研究院 | A kind of method and device for producing feather weight sheet footpath graphite oxide/graphene oxide |
| CN105836737B (en) * | 2016-05-06 | 2018-11-09 | 上海利物盛企业集团有限公司 | A method of it is combined with jet stream stripping using ultrasound stripping and prepares graphene |
| CN105836743B (en) * | 2016-06-21 | 2018-01-30 | 烟台市烯能新材料股份有限公司 | A kind of preparation facilities of graphene powder and preparation method thereof |
-
2017
- 2017-07-03 CN CN201710536333.XA patent/CN107161993B/en active Active
Also Published As
| Publication number | Publication date |
|---|---|
| CN107161993A (en) | 2017-09-15 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN107161993B (en) | High concentration graphene slurry and preparation method thereof and device | |
| CN102532939B (en) | Preparation method of water-based self-dispersion nano organic pigment powder | |
| CN108276854A (en) | Phase-change microcapsule and its preparation method and application | |
| CN106519222A (en) | A graphene/magnetic particle/polyaniline composite porous wave-absorbing material and a preparing method thereof | |
| CN101418137B (en) | Method for preparing ultrafine organic pigment/polymer compound powder by using in-situ polymerization | |
| CN103408968B (en) | A kind of blue disperse dye mixture | |
| CN103203192B (en) | A kind of method of non-ionic reverse micelle system and modified polar material thereof | |
| CN106450330B (en) | A kind of special isomery graphene conductive agent of lithium battery and preparation method thereof | |
| CN107950526A (en) | A kind of broad-spectrum pesticide aqueous suspension agent dispersant and preparation method thereof | |
| CN107686539A (en) | A kind of polycarboxylate water-reducer of ether-ether copolymerization and preparation method thereof | |
| CN102504595B (en) | Azo dye composition, preparation method thereof and use method thereof | |
| CN106848320A (en) | A kind of battery cathode slurry and preparation method thereof | |
| CN103193411A (en) | Modified aliphatic high-efficiency water reducing agent prepared from CLT acid production wastewater as raw material and preparation method of water reducing agent | |
| CN102408562A (en) | Preparation method for polyaniline/ferroferric oxide compound with nucleus-shell structure | |
| CN106084225A (en) | A kind of heavy metal chelant and preparation method thereof | |
| CN111567517B (en) | Novel aqueous pesticide suspending agent and preparation method thereof | |
| CN104087017A (en) | Preparation method of orange disperse dye | |
| CN107910546A (en) | A kind of lithium ion battery positive electrode uniform sizing material preparation method | |
| CN109796815B (en) | Preparation method of graphene modified styrene-acrylic emulsion | |
| CN105165841B (en) | A kind of mesotrione and atrazine composition aqueous suspension agent and preparation method thereof | |
| CN209663066U (en) | A kind of Combined stirring paddle | |
| CN113350523A (en) | Fat oil inclusion compound and preparation method thereof | |
| CN100402205C (en) | Process for preparing nano-nickel powder | |
| CN114982751B (en) | Production process of pesticide water dispersible granule with good stability | |
| CN110436447A (en) | A kind of glue type graphene aqueous slurry 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 | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |