CN105778571B - A kind of graphene composite mortar and preparation method thereof - Google Patents
A kind of graphene composite mortar and preparation method thereof Download PDFInfo
- Publication number
- CN105778571B CN105778571B CN201410815986.8A CN201410815986A CN105778571B CN 105778571 B CN105778571 B CN 105778571B CN 201410815986 A CN201410815986 A CN 201410815986A CN 105778571 B CN105778571 B CN 105778571B
- Authority
- CN
- China
- Prior art keywords
- graphene
- preparation
- oligomer
- mixture
- graphene composite
- 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
Abstract
The present invention provides a kind of preparation method of graphene composite mortar, it includes the following steps：Disperse graphene in decentralized medium A1, obtain mixture B1；Dispersing aid is added in the mixture A1 and the oligomer of phenylamine derivative for being combined with graphene formation π π obtains mixture B2；Mixture B2 is dried to the graphene composite powder that oligomer of phenylamine Derivatives Modified is made and is modified；Graphene composite powder is scattered in decentralized medium A2 and obtains the graphene composite mortar.
Description
Technical field
The present invention relates to a kind of graphene-based slurry and preparation method thereof, more particularly to a kind of oligomer of phenylamine derivative to repair
Adorn modified graphene composite mortar and preparation method thereof.
Background technology
The hexangle type that graphene is made of carbon atom is in honeycomb lattice material, only a carbon atom thickness.Graphene
It was found in 2004, and obtains Nobel Prize in physics in 2010.The monatomic nanostructured of graphene assigns its many and is difficult
The special performance of rival.1. electric conductivity is extremely strong：Electronics in graphene due to not having quality, the movement velocity energy of its electronics substantially
Enough reach the 1/300 of the light velocity, therefore possess superpower electric conductivity.2. superhigh intensity：Graphene hardness is also higher than diamond, but
Possess good toughness, and can bend.3. extra specific surface area：The specific surface area of preferable single-layer graphene can reach
2630m2/ g, and the specific surface area of common activated carbon is 1500m2/ g, the specific surface area of super large make it that graphene is huge as potentiality
Big energy storage material.Exactly because graphene has many excellent performances, the graphene research and development upsurge in global range is excited.
In the recent period, many researchs all concentrate on the synthesis of large scale, Large-scale graphene.At present, the preparation method of graphene
Generally include the methods of mechanical stripping, chemical vapor deposition, oxidationreduction, solution ultrasound are peeled off.But obtained graphene due to
π-πconjugation and Van der Waals force suction-operated and be easy to reunite.Further, since the structure of graphene uniqueness cause its be difficult with
Other media occur physically or chemically to act on, and bond strength is not high, and application field is limited.Therefore, limitation graphene application at present
Maximum bottleneck be how to obtain the modified graphene composite mortar being easily dispersed of stabilization to give full play to its unique thing
Physicochemical performance.
The content of the invention
In view of the deficiencies of the prior art, it is a primary object of the present invention to provide a kind of oligomer of phenylamine Derivatives Modified
Graphene composite mortar and preparation method thereof, the graphene composite mortar not only have good redispersibility, can also be with it
Its medium combines so that graphene is readily dispersed in base material or coated on substrate surface, improves the application of graphene.
A kind of preparation method of graphene composite mortar, it includes the following steps：Disperse graphene in decentralized medium A1
In, obtain mixture B1；Dispersing aid is added in the mixture B1 and for forming the aniline that strong π-π are combined with graphene
Oligomer derivative, make oligomer of phenylamine derivative be uniformly mixed with graphene and oligomer of phenylamine derivative and graphene it
Between formed pi-pi bond obtain mixture B2；The graphene that mixture B2 is dried to obtained oligomer of phenylamine Derivatives Modified modification is answered
Close powder；Graphene composite powder is scattered in decentralized medium A2 and obtains the graphene composite mortar.
Wherein, the decentralized medium A1 and decentralized medium A2 are deionized water, ethanol, acetone, isopropanol, butanol, acetic acid
One or more of mixed solvents in ethyl ester, toluene, chloroform, dimethylformamide, dimethyl sulfoxide (DMSO) dichloroethanes, the graphite
The mass ratio of alkene and the decentralized medium A1 are 1:10~1:10000.
Wherein, the mass ratio of the graphene and the decentralized medium A1 are 1:20~1:1000.
Wherein, the dispersing aid is silane coupling agent, polyvinyl alcohol, polyvinylpyrrolidone, organically-modified poly- silica
Alkane dipropylene glycol monomethyl ether solution, organic silicon surfactant and/or fluorine-containing surfactant, the dispersing aid and mixture
The mass percent (0.01-1) of B1：100.
Wherein, the oligomer of phenylamine derivative is with carboxyl, alkyl, sulfonic group, phosphate, epoxide group, poly- second
The oligomer of phenylamine of glycol group and/or polyvinyl alcohol group.
Wherein, the mass percent of the oligomer of phenylamine derivative and mixture B1 is (0.05-5)：100.
Wherein, the oligomer of phenylamine is aniline tripolymer, Tetraaniline, aniline pentamer, six aggressiveness of aniline, aniline
One kind or combination in eight aggressiveness.
Wherein, the graphene composite powder is disperseed by the process for dispersing of high-speed stirred, ultrasound, ball milling and/or sand milling
In decentralized medium A2.
Wherein, the graphene includes graphene nanometer sheet, graphene micron film, graphene nanobelt, few layer graphene
With multi-layer graphene.
The present invention also provides one kind graphene composite mortar according to made from above-mentioned preparation method.
The preparation method of graphene composite mortar provided by the invention, preparation process innovation, is derived by oligomer of phenylamine
The modification of thing, can effectively improve the dispersiveness and chemical stability of graphene so that graphene is readily dispersed in base
In material or coated on substrate surface, the application of graphene is improved.
Brief description of the drawings
Fig. 1 is answered for comparative example 1 using undressed graphene dispersion in the obtained graphenes of different decentralized medium A2
Closing the photo of slurry, (wherein decentralized medium A2 is specially water (left side), ethanol (in) and tetrahydrofuran (right side))；
Fig. 2 is the graphite that comparative example 2 is obtained using the graphene dispersion Jing Guo Ethanol Treatment in different decentralized medium A2
(wherein decentralized medium A2 is specially water (left side), ethanol (in) and tetrahydrofuran (right side)) to the photo of alkene composite mortar；
By the photo of 1-3 of the embodiment of the present invention graphene composite mortars provided, (wherein, left figure corresponds to embodiment to Fig. 3
1, middle figure corresponds to embodiment 2, and right figure corresponds to embodiment 3)；
The TEM photos for the graphene composite mortar that Fig. 4 is provided by the embodiment of the present invention 1 and 3.It is (wherein, water-based to correspond to
Embodiment 1, oiliness correspond to embodiment 3)
Fig. 5 is Raman collection of illustrative plates (its of graphene composite powder and the undressed graphene of comparative example 1 in embodiment 1
In, solid line represents graphene composite powder described in embodiment 1, and dotted line represents 1 undressed graphene of comparative example).
Embodiment
Graphene composite mortar provided by the invention and preparation method thereof is described further below with reference to attached drawing.
The embodiment of the present invention provides a kind of preparation method of graphene composite mortar, it includes the following steps：
(1) preparation of graphene composite powder：
Process (1)：Disperse graphene in decentralized medium A1, obtain mixture B1.The structure of the graphene is unlimited, its
Including graphene nanometer sheet, graphene micron film, graphene nanobelt, few layer graphene (2-5 layers), multi-layer graphene (2-9
Layer), the derivative of graphene quantum dot and these graphite alkenes materials).The definition of the grapheme material can be found in document
“All in the graphene family–A recommended nomenclature for two-dimensional
carbon materials”.The grapheme material is also selected from thickness≤20nm, it is highly preferred that the material of thickness≤10nm
Material.In the present embodiment, the grapheme material thickness preferably≤3nm, grapheme material is thinner, and pliability is better, easier
Processing.The preparation method of the grapheme material is unlimited, using graphene product well known to those skilled in the art or with often
It is prepared by the preparation method of rule.Grapheme material can be selected from chemical oxidization method such as Brodie methods, Hummers methods or
Graphene oxide prepared by any one method in Staudenmaier methods is through grapheme material made from thermal expansion.Can also
Select mechanical stripping, the grapheme material that liquid phase is peeled off or prepared by electrochemical stripping.The decentralized medium A1 is deionized water, second
One in alcohol, acetone, isopropanol, butanol, ethyl acetate, toluene, chloroform, dimethylformamide, dimethyl sulfoxide (DMSO) dichloroethanes
Kind or several mixed solvents.The mass ratio of the graphene and the decentralized medium A1 are 1:10~1:10000.In order to avoid working as
Graphene content is too low, its application value is little, and when graphene too high levels, oligomer of phenylamine derivative is to its scattered effect
Fruit is limited, it is preferable that the mass ratio of the graphene and the decentralized medium A1 are 1:20~1:1000.
Process (2)：Dispersing aid is added in the mixture B1 and for forming the aniline that strong π-π are combined with graphene
Oligomer derivative, make oligomer of phenylamine derivative be uniformly mixed with graphene and oligomer of phenylamine derivative and graphene it
Between formed pi-pi bond obtain mixture B2.Specifically, the oligomer of phenylamine derivative has good dissolubility, institute is dissolved in
State in decentralized medium.Since the phenyl ring in the oligomer of phenylamine derivative and graphene-structured are close, thus the aniline is low
Polymers derivative can form pi-pi bond between graphene and realize and be mixed with graphene uniform.The dispersing aid may be such that institute
Stating oligomer of phenylamine derivative has more preferable dissolubility, and is mixed evenly with graphene.It is pointed out that utilize aniline
Pi-pi bond is formed between oligomer derivative and graphene, this mode is different from grafting modification, it does not destroy graphene
The structure of itself, also different from the macromolecule of physical coated graphite alkene, it does not sacrifice the performance of graphene.That is,
By oligomer of phenylamine Derivatives Modified modified graphene, it only makes the dispersiveness of graphene and stability more preferable, and does not break
The structure of bad graphene, does not reduce the original performance of graphene yet.
The oligomer of phenylamine derivative is used for graphene powder described in modification.Further, the aniline is oligomeric
Thing derivative is combined with graphene by forming strong pi-pi bond, so as to reduce the surface energy of the graphene, graphene is greatly improved
Dispersiveness and chemical stability so that the graphene is readily dispersed in base material or coated on substrate surface, improves stone
The application of black alkene.
The oligomer of phenylamine derivative is the oligomer of phenylamine with functional group, the functional group include carboxyl, alkyl,
Sulfonic group, phosphate, epoxide group, polyethylene group and/or polyvinyl alcohol group.Preferably, the oligomer of phenylamine is
Aniline tripolymer, Tetraaniline, aniline pentamer, six aggressiveness of aniline, one kind in eight aggressiveness of aniline or combination.Preferably,
The mass percent of the oligomer of phenylamine derivative and mixture B1 is (0.05-5)：100.
Described oligomer of phenylamine or derivatives thereof can have following structural formula：
(M is mainly sodium ion, potassium ion, quaternary ammonium salt etc.).
The dispersing aid can also be used to be more uniformly distributed the scattered of graphene.Preferably, the dispersing aid is silane
Coupling agent, polyvinyl alcohol, polyvinylpyrrolidone, organic modified polyorganosiloxane dipropylene glycol monomethyl ether solution, organosilyl surface
Activating agent and/or fluorine-containing surfactant.The dispersing aid and the mass percent (0.01-1) in mixture B1：100.
Process (3)：Mixture B2 is dried to the graphene composite powder that oligomer of phenylamine Derivatives Modified is made and is modified.It is dry
In graphene composite powder after dry, mass percent of the oligomer of phenylamine derivative in graphene composite powder is
0.1%~50%.
Process (4)：Graphene composite powder is scattered in decentralized medium A2 and obtains the graphene composite mortar.It is described
The mass ratio of graphene powder and the decentralized medium A2 are 1:10~1:10000.Preferably, the graphene powder with it is described
The mass ratio of decentralized medium A2 is 1:20~1:1000.The decentralized medium A2 is identical with decentralized medium A1, and details are not described herein.
It is appreciated that in order to help graphene composite powder preferably to disperse, a dispersant can be also added.The dispersant can be to be modified
Acrylic acid dispersant, polyacrylic acid dipersant, modified poly ester dispersant, polyvinyl alcohol dispersant or modified polyurethane dispersant
Deng.
To further describe the present invention, here is the preparation method of the graphene composite mortar, under different parameters
Specific embodiment：
Embodiment 1：
(1) preparation of graphene composite powder：
Take each component quality as follows：
Graphene (individual layer), 2g；
Deionized water (decentralized medium A1), 98g；
Aniline tripolymer carboxylic acid derivates (carboxyl group, dressing agent), 1g；
Polyvinylpyrrolidone (dispersing aid), 0.05g.
First by graphene and decentralized medium A1, high-speed stirred disperses 20min, and ultrasonic disperse under 1500rad/min
20min, obtains mixture B1.Dispersing aid and aniline tripolymer carboxylic acid derivates are added in mixture B1 again, in high-speed stirring
Mix and stir 2h, then centrifugation at 70 DEG C of constant temperature on machine, obtain mixture B2.Mixture B2 is dried in vacuo at 60 DEG C and is obtained
The graphene composite powder that aniline tripolymer carboxylic acid derivates are modified；
(2) preparation of graphene composite mortar：
Take each component quality as follows：
Obtained graphene composite powder in the present embodiment (1), 5g；
Ethanol, 94.95g；
Modified propylene acid dispersant, 0.05g.
Graphene composite powder is added into ethanol high speed and stirs pre-dispersed 5min, modified propylene acid dispersant is added and surpasses
Sound disperses 30min, and the stir process 1h on homogenizer, obtains graphene composite mortar.
Obtained graphene composite powder and graphene composite mortar are tested for the property, to observe the graphite
The surface characteristic of alkene composite granule and the stability of graphene composite mortar.Obtained graphene composite mortar in the present embodiment
Main performance be shown in Table 1, Fig. 3 and Fig. 4.
Embodiment 2：
(1) preparation of graphene composite powder：
Take each component quality as follows：
Graphene (multilayer), 5g；
Ethanol (decentralized medium A1), 95g；
Tetraaniline alkyl derivative (contains alkyl group, dressing agent), 3g；
Polyvinyl alcohol (dispersing aid), 0.1g.
First by graphene and decentralized medium A1, high-speed stirred disperses 20min, and ultrasonic disperse under 1000rad/min
30min, obtains mixture B1.Dispersing aid and Tetraaniline alkyl derivative are added in mixture B1 again, in high-speed stirring
Mix and stir 2h, then centrifugation at 80 DEG C of constant temperature on machine, obtain mixture B2.Mixture B2 is dried in vacuo at 60 DEG C and is obtained
The graphene composite powder that Tetraaniline alkyl derivative is modified；
(2) preparation of graphene composite mortar：
Take each component quality as follows：
Obtained graphene composite powder in the present embodiment (1), 2g；
Deionized water, 97.95g；
Polyacrylic acid dipersant, 0.05g.
Graphene composite powder is added into deionized water high speed and stirs pre-dispersed 10min, adds polyacrylic acid salinity
Powder ultrasonic disperse 30min, the stir process 1h on homogenizer, obtains graphene composite mortar.
Obtained graphene composite powder and graphene composite mortar are tested for the property, to observe the graphite
The surface characteristic of alkene composite granule and the stability of graphene composite mortar.Obtained graphene composite mortar in the present embodiment
Main performance be shown in Table 1 and Fig. 3.
Embodiment 3：
(1) preparation of graphene composite powder：
Take each component quality as follows：
Graphene (individual layer), 1g；
Acetone (decentralized medium A1), 99g；
Aniline pentamer sulfonic acid radical derivative (contains sulfonic group, dressing agent), 0.5g
Silane coupling agent (dispersing aid), 0.3g.
First by graphene and decentralized medium A1, high-speed stirred disperses 10min, and ultrasonic disperse under 1500rad/min
20min, obtains mixture B1.Dispersing aid and aniline pentamer sulfonic acid radical derivative are added in mixture B1 again, at a high speed
2h, then centrifugation are stirred at 80 DEG C of constant temperature on mixer, obtains mixture B2.Mixture B2 is dried in vacuo at 70 DEG C
The graphene composite powder derivative modified to aniline pentamer sulfonic group；
(2) preparation of graphene composite mortar：
Take each component quality as follows：
Obtained graphene composite powder in the present embodiment (1), 1g；
Ethyl acetate, 98.9g；
Modified poly ester dispersant, 0.1g.
Graphene composite powder is added into ethyl acetate high speed and stirs pre-dispersed 5min, adds modified poly ester dispersant
Ultrasonic disperse 20min, the stir process 1h on homogenizer, obtains graphene composite mortar.
Obtained graphene composite powder and graphene composite mortar are tested for the property, to observe the graphite
The surface characteristic of alkene composite granule and the stability of graphene composite mortar.Obtained graphene composite mortar in the present embodiment
Main performance be shown in Table 1, Fig. 3 and Fig. 4.
Embodiment 4：
(1) preparation of graphene composite powder：
Take each component quality as follows：
Graphene (multilayer), 0.5g；
Toluene (decentralized medium A1), 99.5g；
Six aggressiveness phosphoric acid radical derivative (phosphorous acid group, dressing agent) of aniline, 0.1g；
Organic silicon surfactant (dispersing aid), 0.5g；
First by graphene and decentralized medium A1, high-speed stirred disperses 20min, and ultrasonic disperse under 1500rad/min
10min, obtains mixture B1.Dispersing aid and six aggressiveness phosphoric acid radical derivative of aniline are added in mixture B1 again, at a high speed
2h, then centrifugation are stirred at 80 DEG C of constant temperature on mixer, obtains mixture B2.Mixture B2 is dried in vacuo at 60 DEG C
The graphene composite powder derivative modified to six aggressiveness phosphate of aniline；
(2) preparation of graphene composite mortar：
Take each component quality as follows：
Obtained graphene composite powder in the present embodiment (1), 0.5g；；
Isopropanol, 99g；
Polyvinyl alcohol dispersant, 0.5g.
Graphene composite powder is added into isopropanol high speed and stirs pre-dispersed 5min, polyvinyl alcohol dispersant is added and surpasses
Sound disperses 30min, and the stir process 30min on homogenizer, obtains graphene composite mortar.
Obtained graphene composite powder and graphene composite mortar are tested for the property, to observe the graphite
The surface characteristic of alkene composite granule and the stability of graphene composite mortar.Obtained graphene composite mortar in the present embodiment
Main performance be shown in Table 1.
Embodiment 5：
(1) preparation of graphene composite powder：
Take each component quality as follows：
Graphene (individual layer), 0.1g；
Chloroform (decentralized medium A1), 99.9g；
Eight aggressiveness polyvinyl alcohol radical derivative (group containing polyvinyl alcohol, dressing agent) of aniline, 0.05g；
Organofluoro surfactants (dispersing aid), 0.1g.
First by graphene and decentralized medium A1, high-speed stirred disperses 10min, and ultrasonic disperse under 1500rad/min
10min, obtains mixture B1.Dispersing aid and eight aggressiveness polyvinyl alcohol radical derivative of aniline are added in mixture B1 again,
2h, then centrifugation are stirred at 80 DEG C of constant temperature on homogenizer, obtains mixture B2.By mixture B2, vacuum is done at 70 DEG C
It is dry to obtain the derivative modified graphene composite powder of eight aggressiveness polyvinyl alcohol based of aniline；
(2) preparation of graphene composite mortar：
Take each component quality as follows：
Obtained graphene composite powder in the present embodiment (1), 0.1g；
Toluene, 99g；
Modified polyurethane dispersant, 0.9g.
Graphene composite powder is added into toluene high speed and stirs pre-dispersed 5min, adds a point modified polyurethane dispersant
Ultrasonic disperse 10min, the stir process 20min on homogenizer, obtains graphene composite mortar.
Obtained graphene composite powder and graphene composite mortar are tested for the property, to observe the graphite
The surface characteristic of alkene composite granule and the stability of graphene composite mortar.Obtained graphene composite mortar in the present embodiment
Main performance be shown in Table 1.
In order to contrast the performance of the graphene composite powder prepared by the application, following comparative example 1 and contrast will be also carried out
The experiment of example 2.
Comparative example 1
Take each component quality as follows：
Undressed graphene powder, 0.1g；
Toluene, 99g；
Dispersant, 0.9g.
Undressed graphene powder is separately added into different decentralized medium A2 high speeds and stirs pre-dispersed 5min, then
Dispersant ultrasonic disperse 10min, the stir process 20min on homogenizer are added, obtains three kinds of graphene composite mortars.Its
In, decentralized medium A2 is water, ethanol and tetrahydrofuran.
Undressed graphene powder and graphene slurry are tested for the property, it is described undressed to observe
The surface characteristic of graphene powder and the stability of graphene slurry, results of property are shown in Table 1 and Fig. 1.
Comparative example 2
First by graphene and silane coupling agent, high-speed stirred disperses 20min, and ultrasonic disperse under 1500rad/min
20min, obtains mixture.Mixture is dried in vacuo at 60 DEG C and obtains the graphene powder handled through silane coupling agent.
The graphene powder (0.1g) handled through silane coupling agent is separately added into different decentralized medium A2 (99g) high
Speed stirs pre-dispersed 5min, adds dispersant (0.9g) ultrasonic disperse 10min, stir process 20min on homogenizer,
Obtain three kinds of graphene composite mortars.Wherein, decentralized medium A2 is water, ethanol and tetrahydrofuran.
The graphene powder handled through silane coupling agent and obtained graphene slurry are tested for the property, with observation
The surface characteristic of graphene powder and the stability of graphene slurry handled through silane coupling agent, results of property are shown in Table 1
And Fig. 3.
Table 1 (wherein stability refers to store obtained graphene composite mortar 3 months and observes again)
With reference to Fig. 1-4 and table 1 as can be seen that compared to comparative example 1 using the graphene powder without any processing and
For the graphene slurry that the graphene powder that comparative example 2 is handled merely through silane coupling agent is prepared, using institute of the present invention
The dispersiveness and stability for stating the graphene composite mortar made from preparation method are significantly improved, and can also pass through
The different oligomer of phenylamine derivative of performance and dispersing aid is selected to adjust the surface characteristic of the graphene composite powder
For amphipathic property, so as to be more advantageous to commercial application.
As seen from Figure 5, derive relative to undressed graphene, the graphene composite powder by oligomer of phenylamine
In 1410cm after thing modification-1There is the absworption peak corresponding to pi-pi bond, this demonstrate that in oligomer of phenylamine derivative and graphite
There are pi-pi bond between alkene.
The explanation of above example is only intended to help to understand method and its core concept of the invention.It should be pointed out that pair
For those skilled in the art, without departing from the principle of the present invention, the present invention can also be carried out
Some improvement and modification, these are improved and modification is also fallen into the protection domain of the claims in the present invention.To these embodiments
A variety of modifications are it will be apparent that the general principles defined herein can be not for those skilled in the art
Realized in other embodiments in the case of departing from the spirit or scope of the present invention.Therefore, the present invention is not intended to be limited to this
These embodiments shown in text, and it is to fit to the most wide scope consistent with the principles and novel features disclosed herein.
Claims (9)
1. a kind of preparation method of graphene slurry, it includes the following steps：
Disperse graphene in decentralized medium A1, obtain mixture B1；
Dispersing aid is added in the mixture B1 and for forming the oligomer of phenylamine derivative that strong π-π are combined with graphene
Thing, makes oligomer of phenylamine derivative be uniformly mixed with graphene and π-π is formed between oligomer of phenylamine derivative and graphene
Key obtains mixture B2, wherein, the oligomer of phenylamine is aniline tripolymer, Tetraaniline, aniline pentamer, aniline six are poly-
Body, one kind in eight aggressiveness of aniline or combination；
Mixture B2 is dried to the graphene composite powder that oligomer of phenylamine Derivatives Modified is made and is modified；
Graphene composite powder is scattered in decentralized medium A2 and obtains the graphene slurry.
2. the preparation method of graphene slurry according to claim 1, it is characterised in that the decentralized medium A1 and scattered Jie
Matter A2 is deionized water, ethanol, acetone, isopropanol, butanol, ethyl acetate, toluene, chloroform, dimethylformamide, dimethyl are sub-
One or more of mixed solvents in sulfone, dichloroethanes, the mass ratio of the graphene and the decentralized medium A1 for 1: 10~
1∶10000。
3. the preparation method of graphene slurry according to claim 2, it is characterised in that the graphene and scattered Jie
The mass ratio of matter A1 is 1: 20~1: 1000.
4. the preparation method of graphene slurry according to claim 1, it is characterised in that the dispersing aid is silane coupled
Agent, polyvinyl alcohol, polyvinylpyrrolidone, organic modified polyorganosiloxane dipropylene glycol monomethyl ether solution, organosilicone surfactant
Agent and/or fluorine-containing surfactant, the mass percent (0.01-1) of the dispersing aid and mixture B1: 100.
5. the preparation method of graphene slurry according to claim 1, it is characterised in that the oligomer of phenylamine derivative is
Aniline with carboxyl, alkyl, sulfonic group, phosphate, epoxide group, polyethylene group and/or polyvinyl alcohol group is oligomeric
Thing.
6. the preparation method of graphene slurry according to claim 5, it is characterised in that the oligomer of phenylamine derivative with
The mass percent of mixture B1 is (0.05-5): 100.
7. the preparation method of graphene slurry according to claim 1, it is characterised in that the graphene composite powder passes through
High-speed stirred, ultrasound, the process for dispersing of ball milling and/or sand milling are scattered in decentralized medium A2.
8. the preparation method of graphene slurry according to claim 1, it is characterised in that the graphene is received including graphene
Rice piece, graphene micron film, graphene nanobelt, few layer graphene and multi-layer graphene.
A kind of 9. graphene slurry made from preparation method according to any one of claim 1-8.
Priority Applications (5)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410815986.8A CN105778571B (en) | 2014-12-24 | 2014-12-24 | A kind of graphene composite mortar and preparation method thereof |
| PCT/CN2015/095742 WO2016086796A1 (en) | 2014-12-02 | 2015-11-27 | Graphene dispersant and application thereof |
| TW104139658A TWI602611B (en) | 2014-12-02 | 2015-11-27 | Graphene dispersant and its application |
| EP15865917.7A EP3228592A4 (en) | 2014-12-02 | 2015-11-27 | Graphene dispersant and application thereof |
| US15/607,552 US10696790B2 (en) | 2014-12-02 | 2017-05-29 | Graphene dispersant and application thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410815986.8A CN105778571B (en) | 2014-12-24 | 2014-12-24 | A kind of graphene composite mortar and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN105778571A CN105778571A (en) | 2016-07-20 |
| CN105778571B true CN105778571B (en) | 2018-05-04 |
Family
ID=56377481
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410815986.8A Active CN105778571B (en) | 2014-12-02 | 2014-12-24 | A kind of graphene composite mortar and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105778571B (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107722697A (en) * | 2017-10-31 | 2018-02-23 | 洛阳菁洲纳米科技有限公司 | A kind of preparation method of graphene anticorrosive paint |
Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106554479A (en) * | 2016-11-28 | 2017-04-05 | 厦门艾美森新材料科技股份有限公司 | A kind of polyurethane foam and a kind of modified graphite is dilute and its their preparation method |
| CN108793138A (en) * | 2017-04-26 | 2018-11-13 | 中国科学院理化技术研究所 | A kind of preparation method of functionalization graphene slurry |
| CN107129635A (en) * | 2017-04-28 | 2017-09-05 | 上海烯古能源科技有限公司 | The master batch and its synthetic method of high barrier cast polypropylene film can be prepared |
| CN108794999A (en) * | 2018-05-02 | 2018-11-13 | 陕西金瑞烯科技发展有限公司 | A kind of preparation method of graphene terylene composite material master batch and fiber |
| CN109593409B (en) * | 2018-11-26 | 2021-03-19 | 国宏中晶集团有限公司 | Graphene antifouling paint and preparation method thereof |
| CN109762202A (en) * | 2018-11-28 | 2019-05-17 | 宁波墨西科技有限公司 | A kind of functionalization graphene composite anti-static plastic matrix and preparation method thereof |
Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2007011369A2 (en) * | 2004-08-23 | 2007-01-25 | E.I. Dupont De Nemours And Company | Method for preparing cnt/pani dispersions |
| TW201033244A (en) * | 2008-11-20 | 2010-09-16 | Kwang-Suck Suh | CNT-poly(X-4 styrenesulfonate) composites and CNT-conductive polymer composites produced with the same |
| CN102321254A (en) * | 2011-09-30 | 2012-01-18 | 西安交通大学 | Preparation method for high-concentration graphene-polyaniline nanofiber composite dispersion liquid and high-concentration graphene-polyaniline nanofiber composite film |
| CN102695557A (en) * | 2009-11-25 | 2012-09-26 | 日产化学工业株式会社 | Carbon nano-tube dispersant |
| CN102875844A (en) * | 2012-10-15 | 2013-01-16 | 苏州大学 | Modified carbon nano tube and preparation method thereof |
| CN102911531A (en) * | 2012-10-22 | 2013-02-06 | 中国科学院宁波材料技术与工程研究所 | Method for stably dispersing graphene or/and carbon nanotubes in organic solvent |
| CN103059343A (en) * | 2012-10-15 | 2013-04-24 | 苏州大学 | Modified carbon nanotube and preparation method thereof |
| CN103450714A (en) * | 2012-05-24 | 2013-12-18 | 东丽先端材料研究开发（中国）有限公司 | Conductive graphite flake and preparation method thereof |
| CN103613755A (en) * | 2013-10-17 | 2014-03-05 | 河南科技大学 | Graphene/polyaniline nanometer composite material, preparation method and application |
| CN103623741A (en) * | 2013-11-27 | 2014-03-12 | 中国科学院长春应用化学研究所 | Graphene dispersing agent, preparation method thereof and preparation method of graphene |
-
2014
- 2014-12-24 CN CN201410815986.8A patent/CN105778571B/en active Active
Patent Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2007011369A2 (en) * | 2004-08-23 | 2007-01-25 | E.I. Dupont De Nemours And Company | Method for preparing cnt/pani dispersions |
| TW201033244A (en) * | 2008-11-20 | 2010-09-16 | Kwang-Suck Suh | CNT-poly(X-4 styrenesulfonate) composites and CNT-conductive polymer composites produced with the same |
| CN102695557A (en) * | 2009-11-25 | 2012-09-26 | 日产化学工业株式会社 | Carbon nano-tube dispersant |
| CN102321254A (en) * | 2011-09-30 | 2012-01-18 | 西安交通大学 | Preparation method for high-concentration graphene-polyaniline nanofiber composite dispersion liquid and high-concentration graphene-polyaniline nanofiber composite film |
| CN103450714A (en) * | 2012-05-24 | 2013-12-18 | 东丽先端材料研究开发（中国）有限公司 | Conductive graphite flake and preparation method thereof |
| CN102875844A (en) * | 2012-10-15 | 2013-01-16 | 苏州大学 | Modified carbon nano tube and preparation method thereof |
| CN103059343A (en) * | 2012-10-15 | 2013-04-24 | 苏州大学 | Modified carbon nanotube and preparation method thereof |
| CN102911531A (en) * | 2012-10-22 | 2013-02-06 | 中国科学院宁波材料技术与工程研究所 | Method for stably dispersing graphene or/and carbon nanotubes in organic solvent |
| CN103613755A (en) * | 2013-10-17 | 2014-03-05 | 河南科技大学 | Graphene/polyaniline nanometer composite material, preparation method and application |
| CN103623741A (en) * | 2013-11-27 | 2014-03-12 | 中国科学院长春应用化学研究所 | Graphene dispersing agent, preparation method thereof and preparation method of graphene |
Non-Patent Citations (4)
| Title |
|---|
| Large thermoelectric power factor in polyaniline/graphene nanocomposite films prepared by solution-assistant dispersing method;Liming Wang et al.;《Journal of Materials Chemistry A》;20140520;第2卷(第29期);11107-11113 * |
| Non-covalent functionalization of graphene sheets by sulfonated polyaniline;Hua Bai et al.;《Chem. Commun》;20090210(第13期);1667-1669 * |
| Preparation of a graphene oxide–phthalocyanine hybrid through strong π-π interactions;Xuequan Zhang et al.;《CARBON》;20090906;第48卷;211-216 * |
| Preparation of graphene–polyaniline composites by simple chemical procedure and its improved field emission properties;S. Goswami et al.;《CARBON》;20110131;第49卷;2245-2252 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107722697A (en) * | 2017-10-31 | 2018-02-23 | 洛阳菁洲纳米科技有限公司 | A kind of preparation method of graphene anticorrosive paint |
Also Published As
| Publication number | Publication date |
|---|---|
| CN105778571A (en) | 2016-07-20 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105778571B (en) | A kind of graphene composite mortar and preparation method thereof | |
| JP6208364B2 (en) | Graphene production method and graphene dispersion composition | |
| JP5933374B2 (en) | Method for producing thin-layer graphite or thin-layer graphite compound | |
| CN108706575B (en) | Preparation method of liquid-phase ball-milling stripped graphene | |
| CN104495826B (en) | Single-layer graphene dispersion liquid and preparation method thereof | |
| CN105645388B (en) | Graphene dispersion agent and its application | |
| Dong et al. | A novel fabrication of graphene by chemical reaction with a green reductant | |
| He et al. | Urea-assisted aqueous exfoliation of graphite for obtaining high-quality graphene | |
| US10472243B2 (en) | Industrial method for preparing large-sized graphene | |
| JP6304988B2 (en) | Method for producing graphene sheet organic dispersion, and graphene sheet organic dispersion and heat dissipation graphene sheet structure obtained thereby | |
| JP5995523B2 (en) | Graphene sheet aqueous dispersion, production method thereof, and graphene-containing structure | |
| CN105315476B (en) | A kind of method for preparing modified graphene polyvinyl alcohol compound film | |
| CN106009787B (en) | A kind of classification dispersion method prepares the method and device of graphene aqueous liquid dispersion | |
| WO2016040599A1 (en) | Process for exfoliation and dispersion of boron nitride | |
| CN107200319A (en) | One kettle way liquid phase peels off the method for being prepared on a large scale high-quality graphene | |
| CN107857259A (en) | A kind of method that full carbon face oxidation prepares the dispersible functionalization graphene of low oxygen content | |
| JP5800678B2 (en) | Nanocarbon aqueous dispersion, method for producing the same, and nanocarbon-containing structure | |
| Lu et al. | Aqueous soluble boron nitride nanosheets via anionic compound-assisted exfoliation | |
| CN107365259A (en) | Molybdenum disulfide dispersant, molybdenum disulfide dispersion, its preparation method and application | |
| CN106276881B (en) | A kind of preparation method of graphene | |
| Namvari et al. | Crosslinking hydroxylated reduced graphene oxide with RAFT-CTA: a nano-initiator for preparation of well-defined amino acid-based polymer nanohybrids | |
| CN105788874B (en) | A kind of composite graphite alkene paper and preparation method thereof | |
| CN107364839A (en) | Nitrogenize borated dispersant, liquid phase peels off the method and its application of two-dimentional boron nitride nanosheet | |
| JP6563226B2 (en) | Method for producing flaky carbon | |
| CN105502357B (en) | A kind of mechanical stripping prepares the special remover of Graphene and preparation method |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |