CN109205603A - The dispersing method of graphene - Google Patents
The dispersing method of graphene Download PDFInfo
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- CN109205603A CN109205603A CN201710530097.0A CN201710530097A CN109205603A CN 109205603 A CN109205603 A CN 109205603A CN 201710530097 A CN201710530097 A CN 201710530097A CN 109205603 A CN109205603 A CN 109205603A
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- graphene
- lignin
- dispersing
- dispersing method
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- 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
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/01—Crystal-structural characteristics depicted by a TEM-image
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
Abstract
The invention discloses a kind of dispersing methods of graphene, comprising the following steps: lignin is dissolved in the first solvent, obtains lignin liquor；A certain amount of graphene is added in the lignin liquor, after dispersion, filtering, drying, obtains lignin/graphene composite powder；And the lignin/graphene composite powder is added in one second solvent, dispersion obtains graphene dispersing solution.The present invention is dispersing agent using lignin, realizes the redisperse of graphene, the graphene dispersing solution of available high concentration, high stability.Moreover, the lignin as dispersing agent is from a wealth of sources, belongs to green renewable resource, not will cause environmental pollution.
Description
Technical field
The present invention relates to a kind of dispersing methods of graphene.
Background technique
Graphene is the two-dimensional material with individual layer laminated structure, and thickness only has an atomic diameter size (about
0.35nm), because of its big specific surface area, the features such as high thermal conductivity, low resistivity and impermeability, receives science
The extensive concern on boundary is expected to the revolutionary material as a new generation.But the big specific surface area of graphene and stronger Van der Waals force
Make it that irreversible agglomeration easily occur in dispersing matrixes.It is its excellent property using the basic reason of graphene
Can, these excellent properties can only largely be embodied on monolithic/primary particle, and graphene its performance after reuniting is big
It gives a discount, can even completely lose.In order to improve the dispersion of graphene in water and other solvents, it usually needs some dispersions are added
Agent, such as the small molecule containing aromatic structure or macromolecular or surfactant etc..The dispersing agent includes detergent alkylate sulphur
Sour sodium, 1- pyrene formic acid, 1- pyrene sulfonic acid, how hydrochlorate, lipid surfactant or polyvinylpyrrolidone (PVP) etc..But these
Dispersing agent there is toxicity it is big, dispersion effect is poor, graphene concentration is too low, dispersion stability is poor and higher cost the problems such as.
Summary of the invention
In view of this, the present invention provide it is a kind of low cost, easily preparation, high concentration, high stability graphene dispersion side
Method.
A kind of dispersing method of graphene, comprising the following steps:
(1) lignin is dissolved in the first solvent, obtains lignin liquor；
(2) graphene is added in the lignin liquor, after dispersion, filtering, drying, it is multiple obtains lignin/graphene
Close powder；And
(3) lignin/graphene composite powder is added in one second solvent, dispersion obtains graphene dispersing solution.
Wherein, the lignin is alkaline lignin, dealkalize lignin, lignosulfonates, lignin degrading and phenol
One of hydroformylation lignin is a variety of.
Wherein, first solvent is water, in formaldehyde, acetone, pyridine, ethyl alcohol, tetrahydrofuran, n,N-Dimethylformamide
One or more.
Wherein, second solvent is one or both of water, alkaline solution.
Wherein, the alkaline solution is one or both of aqueous solution and aqueous solution of potassium hydroxide of sodium hydroxide.
Wherein, the concentration of lignin is 0.1mg/mL~50mg/mL in the lignin liquor.
Wherein, the mass ratio of lignin and graphene is 5: 1~1: 1.
Compared with prior art, the present invention is by being dispersed, filtering and doing by the way that graphene to be added in lignin liquor
After dry, lignin/graphene composite powder is obtained, then disperses water or alkalinity for the lignin/graphene composite powder
In solution, the graphene dispersing solution of available high concentration, high stability.
The graphene dispersing solution can be stored 24 hours or more at room temperature.That is, the present invention is dispersing agent using lignin,
Realize the redisperse of graphene.Moreover, the lignin as dispersing agent is from a wealth of sources, belong to green renewable resource, it will not
Cause environmental pollution.In addition, method provided by the present invention is simple, cost is relatively low.
Detailed description of the invention
Fig. 1 is the comparison photo of lignin provided by the invention/graphene composite powder dispersion effect in water.
Fig. 2 is transmission electron microscope (TEM) photo of graphene dispersing solution provided by the invention.
Fig. 3 is scanning probe microscopy (AFM) photo of graphene dispersing solution provided by the invention.
Following specific embodiment will further illustrate the present invention in conjunction with above-mentioned attached drawing.
Specific embodiment
It is described further below with reference to dispersing method of the attached drawing to graphene provided by the invention.
The present invention provides a kind of dispersing method of graphene, comprising the following steps:
(1) lignin is dissolved in the first solvent, obtains lignin liquor；
(2) a certain amount of graphene is added in the lignin liquor, dispersion, filtering, it is dry after, obtain lignin/
Graphene composite powder；
(3) lignin/graphene composite powder is added in one second solvent, dispersion obtains graphene dispersing solution.
In step (1), the lignin role is to contain a large amount of phenyl ring, phenyl ring and graphite in lignin molecule
It forms pi-pi bond cooperation between alkene molecule to use, to can inhibit the agglomeration of graphene.The lignin be alkaline lignin,
One of dealkalize lignin, lignosulfonates, lignin degrading and phenolic aldehyde lignin are a variety of, in order to better
It is bonded lignin with graphene, the lignin is preferably alkaline lignin.First solvent is unlimited, as long as can dissolve institute
State lignin.Preferably, first solvent is water, formaldehyde, acetone, pyridine, ethyl alcohol, tetrahydrofuran, N, N- dimethyl
One or more of formamide.The concentration of lignin is 0.1mg/mL~50mg/mL in the lignin liquor.
In step (2), the average diameter of the graphene is greater than or equal to 10 μm, and the graphene is single layer or few layer
The graphene powder or slurry of (less than 10 layers).The mass ratio of the lignin and graphene is 5: 1~1: 1, it is preferred that described
The mass ratio of lignin and graphene is 2: 1~1: 1.The method of the dispersion is unlimited, can be stirring, ultrasonic disperse etc..It is excellent
Selection of land, first magnetic agitation re-ultrasonic dispersion.The filtering and dry method are unlimited, can take common filtering, dry
Method.
In step (3), second solvent is one of water, alkaline solution or combinations thereof.The alkaline solution is by hydrogen
Obtained by sodium oxide molybdena, potassium hydroxide etc. are dissolved in the water.Therefore, which can be aqueous solution, the hydroxide of sodium hydroxide
The combination of one or more of aqueous solution of potassium etc..The method of the dispersion is unlimited, can be stirring, ultrasonic disperse etc..Institute
The concentration for stating graphene dispersing solution is 0.01mg/mL~20mg/mL.
The present invention is dispersed, after filtering and drying by the way that graphene to be added in lignin liquor, obtains lignin/stone
Then black alkene composite powder disperses the lignin/graphene composite powder in water or alkaline solution, available highly concentrated
The graphene dispersing solution of degree, high stability.The graphene dispersing solution can be stored 24 hours or more at room temperature.That is, of the invention
It is dispersing agent using lignin, realizes the redisperse of graphene.Moreover, the lignin as dispersing agent is from a wealth of sources, belong to
Green renewable resource, not will cause environmental pollution.In addition, method provided by the invention is simple, cost is relatively low.
Hereinafter, will further illustrate in conjunction with specific embodiments.
Embodiment 1
It takes 1.0g alkali lignin to be dissolved in the aqueous solution of 50.0mL sodium hydroxide, 1.0g graphene powder is added.At room temperature
Magnetic agitation for 24 hours after, then 200W ultrasonic disperse 12h, is filtered after being finally neutralized with hydrochloric acid, and filter cake obtains after being dried in vacuo
Lignin/graphene composite powder.
Lignin/graphene composite powder is dispersed in the aqueous solution of sodium hydroxide according to various concentration, ultrasonic disperse
0.5h examines its dispersion effect in the aqueous solution of sodium hydroxide, as shown in table 1.From table 1 it can be seen that, pure graphene powder
It cannot disperse in the aqueous solution of sodium hydroxide, and when lignin/graphene composite powder (pH value 8-10) is in sodium hydroxide
Aqueous solution in concentration be less than or equal to 10mg/mL when, stable graphene can be formed in the aqueous solution of sodium hydroxide
Dispersion liquid.
1. lignin of table/dispersion effect of the graphene composite powder in the aqueous solution of sodium hydroxide
Embodiment 2
It takes 2.0g alkali lignin to be dissolved in 50.0mL formalin, 1.0g graphene powder is added.Magnetic force is stirred at room temperature
After 6h, 200W ultrasonic disperse 12h filters dispersion liquid after isopropanol precipitating, filter cake obtained after being dried in vacuo lignin/
Graphene composite powder.
Lignin/graphene composite powder is added in the aqueous solution of sodium hydroxide according to various concentration, ultrasonic disperse
0.5h examines its dispersion effect in the solution, as shown in table 2.From table 2, it can be seen that, pure graphene powder is in sodium hydroxide
It cannot disperse in aqueous solution, and when lignin/graphene composite powder (pH value 8-10) is in the aqueous solution of sodium hydroxide
When concentration is less than or equal to 15mg/mL, stable graphene dispersing solution can be formed in the aqueous solution of sodium hydroxide.
2. lignin of table/dispersion effect of the graphene composite powder in the aqueous solution of sodium hydroxide
Embodiment 3
It takes 1.0g sodium lignin sulfonate to be dissolved in 50.0mL deionized water, 2.0g graphene powder is added.Magnetic force at room temperature
After stirring 6h, 150W ultrasonic disperse 12h filters dispersion liquid after isopropanol precipitating, and filter cake obtains wood after being dried in vacuo
Quality/graphene composite powder.
Lignin/graphene composite powder is added in deionized water, ultrasonic disperse 0.5h according to various concentration, is examined
Its dispersion effect in the solution, as shown in table 3 and Fig. 1.From table 3 and Fig. 1, it can be seen that, pure graphene powder cannot divide in water
It dissipates, and when the lignin/concentration of graphene composite powder in water is less than or equal to 15mg/mL, it can be formed in water steady
Fixed graphene dispersing solution.
3. lignin of the table/dispersion effect of graphene composite powder in water
Embodiment 4
2mg/mL graphene dispersing solution in embodiment 3 is diluted 20 times, utilizes transmission electron microscope (TEM) and scanning
Probe microscope (AFM) observes the dispersity and the number of plies of graphene in the graphene dispersing solution.The graphene dispersing solution from Fig. 2
TEM result can be seen that graphene transparent fine gauze shape be presented in water, illustrate that graphene dispersion is in good condition.By in Fig. 3
The average thickness that the AFM result of graphene dispersing solution can be seen that graphene in graphene dispersing solution is about 1.5nm, illustrates stone
The dispersion of single layer and few layer is presented in black alkene in water.
The above description of the embodiment is only used to help understand the method for the present invention and its core ideas.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 improvements and modifications, these improvements and modifications also fall within the scope of protection of the claims of the present invention.
The foregoing description of the disclosed embodiments enables those skilled in the art to implement or use the present invention.
Various modifications to these embodiments will be readily apparent to those skilled in the art, as defined herein
General Principle can be realized in other embodiments without departing from the spirit or scope of the present invention.Therefore, of the invention
It is not intended to be limited to the embodiments shown herein, and is to fit to and the principles and novel features disclosed herein phase one
The widest scope of cause.
Claims (10)
1. a kind of dispersing method of graphene, comprising the following steps:
(1) lignin is dissolved in the first solvent, obtains lignin liquor；
(2) graphene is added into the lignin liquor, after dispersion, filtering, drying, it is compound obtains lignin/graphene
Powder；And
(3) lignin/graphene composite powder is added into one second solvent, disperses, obtains graphene dispersing solution.
2. the dispersing method of graphene as described in claim 1, which is characterized in that the lignin is alkaline lignin, takes off
One of alkali lignin, lignosulfonates, lignin degrading and phenolic aldehyde lignin are a variety of.
3. the dispersing method of graphene as described in claim 1, which is characterized in that first solvent is water, formaldehyde, third
One or more of ketone, pyridine, ethyl alcohol, tetrahydrofuran, n,N-Dimethylformamide.
4. the dispersing method of graphene as described in claim 1, which is characterized in that second solvent is water, alkaline solution
One or both of.
5. the dispersing method of graphene as claimed in claim 4, which is characterized in that the alkaline solution is the water of sodium hydroxide
One or both of solution and the aqueous solution of potassium hydroxide.
6. the dispersing method of graphene as described in claim 1, which is characterized in that the average diameter of the graphene be greater than or
Equal to 10 μm.
7. the dispersing method of graphene as described in claim 1, which is characterized in that in the step (2), lignin and graphite
The quality of alkene this be 1: 0.01~1: 10.
8. the dispersing method of graphene as described in claim 1, which is characterized in that in the step (3), graphene dispersing solution
Concentration be 0.01mg/mL~20mg/mL.
9. the dispersing method of graphene as described in claim 1, which is characterized in that in the step (1), lignin liquor is
1.0g sodium lignin sulfonate is dissolved in 50.0mL water and is formed；
In step (2), the graphene of 2.0g is added in the lignin liquor.
10. the dispersing method of graphene as described in claim 1, which is characterized in that in the step (1), by 1.0g alkalinity
Lignin is dissolved in the aqueous solution of 50.0mL sodium hydroxide, obtains the lignin liquor；
In step (2), 1.0g graphene is added in the lignin liquor.
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| CN201710530097.0A CN109205603A (en) | 2017-06-30 | 2017-06-30 | The dispersing method of graphene |
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Cited By (1)
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| CN114671429A (en) * | 2022-04-27 | 2022-06-28 | 深圳材启新材料有限公司 | Preparation method of high-quality graphene dispersion liquid |
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Application publication date: 20190115 |