CN104692374A - Preparation method of high-concentration graphene dispersion - Google Patents
Preparation method of high-concentration graphene dispersion Download PDFInfo
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- CN104692374A CN104692374A CN201510117155.8A CN201510117155A CN104692374A CN 104692374 A CN104692374 A CN 104692374A CN 201510117155 A CN201510117155 A CN 201510117155A CN 104692374 A CN104692374 A CN 104692374A
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Abstract
The invention relates to the field of material preparation, in particular to a preparation method of high-concentration graphene dispersion, and discloses a preparation method of high-concentration and high-stability graphene dispersion through a microwave assisted liquid stripping method and a method for obtaining the graphene dispersion with different concentration gradients through grading dilution to further determine the stability of the graphene dispersion. The preparation method comprises the following steps: (1) preparing oxidized graphene dispersion; (2) preparing the graphene dispersion by the microwave assisted liquid-phase stripping. The high-concentration and high-stability graphene dispersion is prepared, the preparation method is simple, is easy to operate and realize, and can meet the requirement on large-scale production.
Description
Technical field
The present invention relates to field of material preparation, be specifically related to a kind of preparation method of high concentration graphene dispersion liquid.
Background technology
Since Graphene in 2010 obtains the Nobel prize, the high conductivity that Graphene itself has, high thermal conductivity cause extensive concern, and show excellent characteristic at energy storage, environmental area.But because Graphene exists Van der Waals force between layers, be easy to reunite.In actual applications, grapheme material needs to be dispersed in water and all kinds of SOLVENTS, but grapheme material is reunited in a large number, thus make it be difficult to be scattered in all kinds of SOLVENTS, namely dispersion is allowed to, due to the nano effect of Graphene, be also difficult to long-time stable in higher concentrations and exist, greatly limit its application.
The method preparing graphene dispersing solution at present mainly contains two kinds, and one is adopt oxidation reduction process to obtain Graphene, then by later stage Graphene modification, or add tensio-active agent acquisition graphene dispersing solution; Two is adopt liquid phase to peel off, and directly obtains graphene dispersing solution by graphite.First method is owing to adopting oxidation reduction process, and introduce other solvent in reaction, the defect of synthesizing graphite alkene not only can be caused many, and solvent remaining in simultaneous reactions also exists negative impact to subsequent applications, causes its degradation, especially electroconductibility.As can be seen here, the graphene dispersing solution that the method obtains is extremely restricted in its application.And the graphene dispersing solution that second method is obtained by liquid phase stripping method, its graphene-structured is complete, and quality is high.But the method productive rate is low, between Graphene, lack good interface binding power, high concentration graphene dispersion liquid cannot be obtained, be unfavorable for that industrial scale uses.
Summary of the invention
In order to solve the deficiencies in the prior art, the invention provides a kind of by adopting microwave-assisted liquid phase stripping method to obtain high density and the preparation method of the graphene dispersing solution of good stability, and obtain different concns gradient graphene dispersing solution by classification dilution, and then determine the stability of graphene dispersing solution.
The technical solution adopted in the present invention is as follows: a kind of preparation method of high concentration graphene dispersion liquid, comprises the following steps:
(1) graphene oxide dispersion is prepared
After 1g graphite and 20-60mL 98% vitriol oil mixing and stirring, add 4g potassium permanganate, continue to stir 1h, after being then warming up to 40-60 DEG C of reaction 24h, add the frozen water dilution of 0 DEG C; Then fully wash to neutrality with distilled water, ultrasonic stripping 2h, centrifugal treating removing is a small amount of impurity wherein, obtains the graphene oxide colloidal suspensions of isotropic stable, suction filtration is carried out to graphene oxide suspension, is then placed in vacuum drying oven and dries and can obtain graphene oxide and divide powder; Graphene oxide powder is joined in different dispersion agent and obtains graphene oxide dispersion;
(2) microwave-assisted liquid phase is peeled off and is prepared graphene dispersing solution
Graphene oxide dispersion in step (1) is placed in microwave reactor, after 2-10min, obtains graphene suspension, ultrasonic 1h, obtain the graphene dispersing solution of isotropic stable.
In addition, preparing graphene dispersing solution can also be placed in microwave reactor by the graphene oxide dispersion in step (1), obtains graphene suspension after 2-10min, and graphene suspension is static, removes supernatant liquor, and bottom settlings is dried, and weighs; The graphene powder obtained is configured the graphene dispersing solution of different concns according to aimed concn, because microwave method gained Graphene obtains in destination scatter agent atmosphere, very well dispersed when being therefore again dispersed in destination scatter agent, high concentration graphene dispersion liquid can be obtained.
As preferably, described dispersion agent is the solvent that specific inductivity is greater than 15.
As preferably, described dispersion agent is one or more in water, N-Methyl pyrrolidone, dinethylformamide, ethylene glycol, dimethylbenzene, acetone.
As preferably, described graphene oxide dispersion concentration is 0-20mg/ml.
As preferably, the power of described microwave reactor is 100-900W.
The beneficial effect that technical scheme provided by the invention is brought is: the graphene dispersing solution of the present invention by adopting microwave-assisted liquid phase stripping method to obtain high density, the advantage of this preparation method: (1) can quick obtaining Graphene; (2) according to target solvent, obtain the high concentration dispersion be scattered in target solvent, the dispersity avoiding twice dispersing to bring reduces; (3) to graphene-structured without destruction, keep the high conductivity of grapheme material, be beneficial to and play a role at energy field; (4) pollution-free, in preparation process, solvent for use plays three aspect effects, a dispersion solvent, two reduction, and three intercalators, fully ensure comprehensive use of solvent; (5) high concentration graphene dispersion liquid is obtained, due to employing is the mode directly being obtained graphene dispersing solution by graphene oxide, Graphene concentration obtains by regulating graphene oxide concentration, graphene oxide is dispersed high in water, provides prerequisite for obtaining high-concentration stable graphene dispersing solution; (6) big size graphene can be obtained.The present invention not only prepares high density, the good graphene dispersing solution of stability, and preparation method is simple, easy to operate, easily realizes, and can meet scale operation.As can be seen here, compared with prior art, have outstanding substantive distinguishing features and significant progress, its beneficial effect implemented also is apparent in the present invention.
Embodiment
For making the object, technical solutions and advantages of the present invention clearly, below embodiment of the present invention is described further in detail.
Embodiment 1:
(1) graphene oxide dispersion is prepared
After 1g graphite and 20mL 98% vitriol oil mixing and stirring, add 4g potassium permanganate, continue to stir 1h, after being then warming up to 40 DEG C of reaction 24h, add the frozen water dilution of 0 DEG C; Then fully wash to neutrality with distilled water, ultrasonic stripping 2h, centrifugal treating removing is a small amount of impurity wherein, obtains the graphene oxide colloidal suspensions of isotropic stable, suction filtration is carried out to graphene oxide suspension, is then placed in vacuum drying oven and dries and can obtain graphene oxide and divide powder; Joined by graphene oxide powder in dispersion agent dimethylbenzene, obtain graphene oxide dispersion, the concentration of graphene oxide dispersion is 1mg/ml;
(2) microwave-assisted liquid phase is peeled off and is prepared graphene dispersing solution
Graphene oxide dispersion in step (1) is placed in the microwave reactor that power is 100W, obtains graphene suspension after 2min, ultrasonic 1h, obtain the graphene dispersing solution of isotropic stable, the concentration adopting spectrophotometry test dispersion liquid is 0.5mg/ml.
High concentration graphene dispersion stability is tested
Diluted gradually by the graphene dispersing solution of 0.5mg/ml, dilute the graphene dispersing solution for different concns gradient, be diluted to 0.01mg/ml always, the concentration adopting spectrophotometer test graphene dispersing solution is 0.009mg/ml.Prove that 0.5mg/ml graphene dispersing solution is highly stable.
Embodiment 2:
(1) graphene oxide dispersion is prepared
After 1g graphite and 40mL 98% vitriol oil mixing and stirring, add 4g potassium permanganate, continue to stir 1h, after being then warming up to 50 DEG C of reaction 24h, add the frozen water dilution of 0 DEG C; Then fully wash to neutrality with distilled water, ultrasonic stripping 2h, centrifugal treating removing is a small amount of impurity wherein, obtains the graphene oxide colloidal suspensions of isotropic stable, suction filtration is carried out to graphene oxide suspension, is then placed in vacuum drying oven and dries and can obtain graphene oxide and divide powder; Joined by graphene oxide powder in dispersion agent N-Methyl pyrrolidone, obtain graphene oxide dispersion, the concentration of graphene oxide dispersion is 20mg/ml;
(2) microwave-assisted liquid phase is peeled off and is prepared graphene dispersing solution
Graphene oxide dispersion in step (1) is placed in the microwave reactor that power is 400W, obtains graphene suspension after 5min, ultrasonic 1h, obtain the graphene dispersing solution of isotropic stable, the concentration adopting spectrophotometry test dispersion liquid is 15mg/ml.
High concentration graphene dispersion stability is tested
Diluted gradually by the graphene dispersing solution of 15mg/ml, dilute the graphene dispersing solution for different concns gradient, be diluted to 1.5mg/ml always, the concentration adopting spectrophotometer test graphene dispersing solution is 1.49mg/ml.Prove that 15mg/ml graphene dispersing solution is highly stable.
Embodiment 3:
(1) graphene oxide dispersion is prepared
After 1g graphite and 50mL 98% vitriol oil mixing and stirring, add 4g potassium permanganate, continue to stir 1h, after being then warming up to 60 DEG C of reaction 24h, add the frozen water dilution of 0 DEG C; Then fully wash to neutrality with distilled water, ultrasonic stripping 2h, centrifugal treating removing is a small amount of impurity wherein, obtains the graphene oxide colloidal suspensions of isotropic stable, suction filtration is carried out to graphene oxide suspension, is then placed in vacuum drying oven and dries and can obtain graphene oxide and divide powder; Joined by graphene oxide powder in dispersion agent ethylene glycol, obtain graphene oxide dispersion, the concentration of graphene oxide dispersion is 5mg/ml;
(2) microwave-assisted liquid phase is peeled off and is prepared graphene dispersing solution
Graphene oxide dispersion in step (1) is placed in the microwave reactor that power is 400W, obtains graphene suspension after 3min, ultrasonic 1h, obtain the graphene dispersing solution of isotropic stable, the concentration adopting spectrophotometry test dispersion liquid is 3.2mg/ml.
High concentration graphene dispersion stability is tested
Diluted gradually by the graphene dispersing solution of 3.2mg/ml, dilute the graphene dispersing solution for different concns gradient, be diluted to 0.32mg/ml always, the concentration adopting spectrophotometer test graphene dispersing solution is 0.318mg/ml.Prove that 3.2mg/ml graphene dispersing solution is highly stable.
Embodiment 4:
(1) graphene oxide dispersion is prepared
After 1g graphite and 50mL 98% vitriol oil mixing and stirring, add 4g potassium permanganate, continue to stir 1h, after being then warming up to 40 DEG C of reaction 24h, add the frozen water dilution of 0 DEG C; Then fully wash to neutrality with distilled water, ultrasonic stripping 2h, centrifugal treating removing is a small amount of impurity wherein, obtains the graphene oxide colloidal suspensions of isotropic stable, suction filtration is carried out to graphene oxide suspension, is then placed in vacuum drying oven and dries and can obtain graphene oxide and divide powder; Joined by graphene oxide powder in dispersion agent dinethylformamide, obtain graphene oxide dispersion, the concentration of graphene oxide dispersion is 10mg/ml;
(2) microwave-assisted liquid phase is peeled off and is prepared graphene dispersing solution
Graphene oxide dispersion in step (1) is placed in the microwave reactor that power is 600W, obtains graphene suspension after 7min, ultrasonic 1h, obtain the graphene dispersing solution of isotropic stable, the concentration adopting spectrophotometry test dispersion liquid is 8mg/ml.
High concentration graphene dispersion stability is tested
Diluted gradually by the graphene dispersing solution of 8mg/ml, dilute the graphene dispersing solution for different concns gradient, be diluted to 0.8mg/ml always, the concentration adopting spectrophotometer test graphene dispersing solution is 0.79mg/ml.Prove that 8mg/ml graphene dispersing solution is highly stable.
Embodiment 5:
(1) graphene oxide dispersion is prepared
After 1g graphite and 60mL 98% vitriol oil mixing and stirring, add 4g potassium permanganate, continue to stir 1h, after being then warming up to 60 DEG C of reaction 24h, add the frozen water dilution of 0 DEG C; Then fully wash to neutrality with distilled water, ultrasonic stripping 2h, centrifugal treating removing is a small amount of impurity wherein, obtains the graphene oxide colloidal suspensions of isotropic stable, suction filtration is carried out to graphene oxide suspension, is then placed in vacuum drying oven and dries and can obtain graphene oxide and divide powder; Joined by graphene oxide powder in dispersion agent dinethylformamide, obtain graphene oxide dispersion, the concentration of graphene oxide dispersion is 12mg/ml;
(2) microwave-assisted liquid phase is peeled off and is prepared graphene dispersing solution
Graphene oxide dispersion in step (1) is placed in the microwave reactor that power is 900W, obtains graphene suspension after 10min, ultrasonic 1h, obtain the graphene dispersing solution of isotropic stable, the concentration adopting spectrophotometry test dispersion liquid is 10mg/ml.
High concentration graphene dispersion stability is tested
Diluted gradually by the graphene dispersing solution of 10mg/ml, dilute the graphene dispersing solution for different concns gradient, be diluted to 1mg/ml always, the concentration adopting spectrophotometer test graphene dispersing solution is 0.99mg/ml.Prove that 10mg/ml graphene dispersing solution is highly stable.
Comparative example 1
After 1g graphite and 50mL 98% vitriol oil mixing and stirring, add 4g potassium permanganate, continue to stir 1h, after being then warming up to 60 DEG C of reaction 24h, add the frozen water dilution of 0 DEG C; Then fully wash to neutrality with distilled water, ultrasonic stripping 2h, centrifugal treating removing is a small amount of impurity wherein, obtains the graphene oxide colloidal suspensions of isotropic stable, suction filtration is carried out to graphene oxide suspension, is then placed in vacuum drying oven and dries and can obtain graphene oxide and divide powder;
Graphene dispersing solution is prepared in chemical reduction
The graphene oxide aqueous dispersions 100ml of configuration 2mg/ml, adds 2ml hydrazine hydrate after ultrasonic disperse 2h under room temperature, reaction 4h; Use distilled water cleaning and filtering, obtain Graphene; By 0.1g Graphene ultrasonic disperse in 10ml N-Methyl pyrrolidone, leave standstill after ultrasonic 2h and remove bottom settlings, adopt spectrophotometer test Graphene dispersion liquid concentration to be 0.01mg/ml.
Comparative example 2
After 1g graphite and 50mL 98% vitriol oil mixing and stirring, add 4g potassium permanganate, continue to stir 1h, after being then warming up to 60 DEG C of reaction 24h, add the frozen water dilution of 0 DEG C; Then fully wash to neutrality with distilled water, ultrasonic stripping 2h, centrifugal treating removing is a small amount of impurity wherein, obtains the graphene oxide colloidal suspensions of isotropic stable, suction filtration is carried out to graphene oxide suspension, is then placed in vacuum drying oven and dries and can obtain graphene oxide and divide powder;
By the graphene oxide after oven dry, 400 DEG C, under nitrogen protection, reduction obtains Graphene; By 1g Graphene ultrasonic disperse in 100ml N-Methyl pyrrolidone, leave standstill after ultrasonic 2h and remove bottom settlings, adopt spectrophotometer test Graphene dispersion liquid concentration to be 0.05mg/ml.
From embodiment 1-5 and comparative example 1-2, the dispersity of the graphene dispersing solution adopting method of the present invention to prepare is tens and even hundred times of the graphene dispersing solution dispersity prepared by ordinary method, as can be seen here, the present invention has outstanding substantive distinguishing features and significant progress.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, within the spirit and principles in the present invention all, any amendment done, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (5)
1. a preparation method for high concentration graphene dispersion liquid, is characterized in that: comprise the following steps:
(1) graphene oxide dispersion is prepared
After 1g graphite and 20-60mL 98% vitriol oil mixing and stirring, add 4g potassium permanganate, continue to stir 1h, after being then warming up to 40-60 DEG C of reaction 24h, add the frozen water dilution of 0 DEG C; Then fully wash to neutrality with distilled water, ultrasonic stripping 2h, centrifugal treating removing is a small amount of impurity wherein, obtains the graphene oxide colloidal suspensions of isotropic stable, suction filtration is carried out to graphene oxide suspension, is then placed in vacuum drying oven and dries and can obtain graphene oxide and divide powder; Graphene oxide powder is joined in different dispersion agent and obtains graphene oxide dispersion;
(2) microwave-assisted liquid phase is peeled off and is prepared graphene dispersing solution
Graphene oxide dispersion in step (1) is placed in microwave reactor, after 2-10min, obtains graphene suspension, ultrasonic 1h, obtain the graphene dispersing solution of isotropic stable.
2. the preparation method of a kind of high concentration graphene dispersion liquid according to claim 1, is characterized in that: described dispersion agent is the solvent that specific inductivity is greater than 15.
3. the preparation method of a kind of high concentration graphene dispersion liquid according to claim 2, is characterized in that: described dispersion agent is one or more in water, N-Methyl pyrrolidone, dinethylformamide, ethylene glycol, dimethylbenzene, acetone.
4. the preparation method of a kind of high concentration graphene dispersion liquid according to claim 1, is characterized in that: described graphene oxide dispersion concentration is 0-20mg/ml.
5. the preparation method of a kind of high concentration graphene dispersion liquid according to claim 1, is characterized in that: the power of described microwave reactor is 100-900W.
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Cited By (5)
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| CN104961125A (en) * | 2015-06-24 | 2015-10-07 | 上海大学 | Graphene high in solubility and preparation method thereof |
| CN105572209A (en) * | 2015-12-23 | 2016-05-11 | 湖北民族学院 | Method utilizing liquid phase to strip graphene modified electrode to measure content of resveratrol |
| CN108147402A (en) * | 2018-02-21 | 2018-06-12 | 吴亚良 | A kind of preparation method of high-quality graphene material |
| TWI636954B (en) * | 2016-11-16 | 2018-10-01 | 財團法人紡織產業綜合研究所 | Graphene dispersion and preparation method thereof |
| CN108726513A (en) * | 2018-09-05 | 2018-11-02 | 广东墨睿科技有限公司 | A kind of preparation method of graphene dispersing solution |
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| US20130087446A1 (en) * | 2011-10-11 | 2013-04-11 | Aruna Zhamu | One-step production of graphene materials |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104961125A (en) * | 2015-06-24 | 2015-10-07 | 上海大学 | Graphene high in solubility and preparation method thereof |
| CN105572209A (en) * | 2015-12-23 | 2016-05-11 | 湖北民族学院 | Method utilizing liquid phase to strip graphene modified electrode to measure content of resveratrol |
| CN105572209B (en) * | 2015-12-23 | 2018-04-03 | 湖北民族学院 | The method that graphene modified determination of electrode Resveratrol content is peeled off using liquid phase |
| TWI636954B (en) * | 2016-11-16 | 2018-10-01 | 財團法人紡織產業綜合研究所 | Graphene dispersion and preparation method thereof |
| CN108147402A (en) * | 2018-02-21 | 2018-06-12 | 吴亚良 | A kind of preparation method of high-quality graphene material |
| CN108147402B (en) * | 2018-02-21 | 2021-06-25 | 江西中聚宏新材料科技有限公司 | Preparation method of high-quality graphene material |
| CN108726513A (en) * | 2018-09-05 | 2018-11-02 | 广东墨睿科技有限公司 | A kind of preparation method of graphene dispersing solution |
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Application publication date: 20150610 |