CN106430170A - Preparation method of graphene dispersion solution - Google Patents
Preparation method of graphene dispersion solution Download PDFInfo
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- CN106430170A CN106430170A CN201610905006.2A CN201610905006A CN106430170A CN 106430170 A CN106430170 A CN 106430170A CN 201610905006 A CN201610905006 A CN 201610905006A CN 106430170 A CN106430170 A CN 106430170A
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- graphene
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- dispersing solution
- dispersion
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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
- C01B2204/30—Purity
Abstract
The invention discloses a preparation method of a graphene dispersion solution. The preparation method specifically comprises steps as follows: graphene is added to a solvent, ball milling and even mixing are performed, then a graphene mixed solution is dispersed through bath type ultrasonic and mechanical stirring devices, the ultrasonic frequency is adjusted to 30-50 KHz, the electric stirring speed is 1,000-10,000 rpm, the dispersion temperature is adjusted to 20-50 DEG C by an external circulating cooling system, and the graphene dispersion solution is obtained finally. Graphene is dispersed by combining multiple dispersion methods including ball milling, ultrasonic and mechanical stirring, the dispersion time is greatly shortened, the production efficiency is improved, batch production is facilitated, no surfactant is added, and the preparation method has the characteristics of low cost, environment friendliness and the like and is prone to mass production and industrial application.
Description
Technical field
The invention belongs to nano material technology, and in particular to a kind of preparation method of graphene dispersing solution.
Background technology
Graphene is the two dimensional crystal of the only one layer of atomic thickness being made up of carbon atom.The dilute current-carrying at room temperature of graphite
Sub- migration rate is 15000 cm2/ (V.s), far above the carrier mobility speed of CNT under room temperature or silicon, and graphite
Dilute resistivity is about 10-6Ω .cm, lower than copper or silver, it is the material of world resistivity minimum.Under room temperature, graphite is dilute with very
High thermal conductivity, about 5300 W/m.K, high CNT at room temperature and diamond.The dilute Young's moduluss of graphite reach
1 TPa, thus it is described as material most firm in the world.Graphene has light weight, density is low, specific surface area is big, electrical property
The feature of the energy good and high mechanical strength of excellent, heat conductivity and the performance of the uniqueness such as Hall effect and quantum tunneling, extensively should
The fields such as preparation and electronic device, energy storage, catalysis, biosensor for nano composite material.
The process for dispersing of Graphene mainly has physics and two big class of chemical dispersion method at present.Either physical dispersion method is still
Chemical dispersion method has its defect, and such as physical dispersion method can break up big Graphene aggregate, but " the nanometer due to Graphene
Effect ", scattered Graphene is easy to reunite again together.Chemical dispersion method can make Graphene absorption dispersant, lead to
Cross electrostatic force or sterically hindered active force is mutually exclusive, obtain stable graphene dispersing solution.But, divided using chemical method
Surfactant has often been adsorbed on its surface of scattered Graphene, during specific use, as surfactant is difficult to remove
Go, the device performance that can prepare to dispersion liquid and thus brings adverse effect.Therefore, it is easier to keep stone using physical dispersion method
The excellent properties of black alkene, are also more favored in the application.However, being disperseed to Graphene using single one physical means, yield
Low, stability is poor, it is impossible to meet industrialized demand.
Content of the invention
It is an object of the invention to provide a kind of can obtain good dispersion, the graphene dispersion of stable and free from admixture pollution
The preparation method of liquid, to make up the deficiency of single dispersed graphite alkene method at present.
For reaching above-mentioned purpose, the present invention prepares graphene mixed liquor and then by ultrasonic and mechanical initially with ball milling
Stirring finally obtains graphene dispersing solution to mixed liquor decentralized processing.
The present invention is achieved through the following technical solutions：
A kind of preparation method of graphene dispersing solution, which is characterized in that and comprises the following steps：
（1）The Graphene of certain mass is dissolved in solvent so as to which concentration is 0.1 ~ 10.0mg/ml, then ball milling mixing, adjusts
Ball milling speed is 100 ~ 500 rpm, and it is 1 that Ball-milling Time is 0 ~ 6 h, ball material volume ratio:3~1:5；
（2）The Graphene liquid of above-mentioned mix homogeneously is carried out decentralized processing using bath ultrasound and mechanical stirring device, is adjusted super
Acoustic frequency is 30 ~ 50 KHz, electric stirring speed is 1000 ~ 10000 rpm, by external circulation cooling system regulation dispersion temperature
Spend for 20-50 DEG C, through the jitter time of 3～20 h, obtain graphene solution；
（3）With the centrifugal speed of 500 ~ 5000rpm, graphene solution is centrifuged, then takes upper solution therein（About
80%）As graphene dispersing solution.
The preparation method of the graphene dispersing solution of the present invention, step（1）Described solvent be 1-Methyl-2-Pyrrolidone,
The mixed solvent of one or more compositions in DMF, isopropanol, BDO.
Graphene dispersing solution prepared by the present invention measures its actual Graphene by the method for ultraviolet test concentrations
Concentration.
The present invention combines to disperse Graphene by ball milling, ultrasound and the multiple process for dispersing of mechanical agitation, greatly
Shorten jitter time greatly, production efficiency is improve, beneficial to batch production, and any surfactant, tool need not be added
The features such as having with low cost, environmental friendliness, it is easy to large-scale production and industrial applications.
Description of the drawings
Fig. 1 is respectively the graphene dispersing solution that embodiment 1,2,3 is obtained from left to right（Standing 60 days）.
Fig. 2 is respectively the graphene dispersing solution that embodiment 4,5,6 is obtained from left to right（Standing 50 days）.
Specific embodiment
The invention will be further described with reference to embodiments.
Embodiment 1
Weigh 10 mg Graphenes to be dissolved in the 1-Methyl-2-Pyrrolidone of 20 mL, the mixing speed for adjusting motor stirrer is
1500 rpm, keep 40 kHz of supersonic frequency, and keep reaction temperature for 35～45 DEG C, through the jitter time of 5 h, it is possible to
Obtain graphene solution.Graphene dispersing solution being obtained after 2000rpm is centrifuged 1 h, concentration is measured for 0.08 m g/ml.
Embodiment 2
Weigh 10mg Graphene to be dissolved in the 1-Methyl-2-Pyrrolidone of 20mL, the mixing speed for adjusting motor stirrer is
1500rpm, keeps supersonic frequency 40kHz, and keeps reaction temperature for 35～45 DEG C, through the jitter time of 7.5h, it is possible to
Obtain graphene solution.Graphene dispersing solution being obtained after 2000 leave heart 1h, concentration is measured for 0.18mg/ml.
Embodiment 3
Weigh 10mg Graphene to be dissolved in the 1-Methyl-2-Pyrrolidone of 20mL, the mixing speed for adjusting motor stirrer is
1500rpm, keeps supersonic frequency 40kHz, and keeps reaction temperature for 35～45 DEG C, through the jitter time of 10h, it is possible to
To graphene solution.Graphene dispersing solution being obtained after 2000 leave heart 1h, concentration is measured for 0.25mg/ml.
Embodiment 4
Weigh 10mg Graphene to be dissolved in the 1-Methyl-2-Pyrrolidone of 20mL, the mixing speed for adjusting motor stirrer is
2500rpm, keeps supersonic frequency 40kHz, and keeps reaction temperature for 35～45 DEG C, through the jitter time of 10h, it is possible to
To graphene solution.Graphene dispersing solution being obtained after 2000 leave heart 1h, concentration is measured for 0.34mg/ml.
Embodiment 5
Weigh 10 mg Graphenes to be dissolved in the 1-Methyl-2-Pyrrolidone of 20 mL, the mixing speed for adjusting motor stirrer is
5000rpm, keeps 40 kHz of supersonic frequency, and keeps reaction temperature for 35～45 DEG C, through the jitter time of 10h, it is possible to
Obtain graphene solution.Graphene dispersing solution being obtained after 2000 leave heart 1h, concentration is measured for 0.36 mg/ml.
Embodiment 6
Weigh 50 mg Graphenes to be dissolved in the 1-Methyl-2-Pyrrolidone of 50 mL, with 200rpm ball milling 4h, ball and the volume that expects
Than being about 1:3, the mixed liquor after ball milling to be disperseed with dispersal device, the mixing speed for adjusting motor stirrer is
5000rpm, keeps 40 kHz of supersonic frequency, and keeps reaction temperature for 35～45 DEG C, through the jitter time of 10h, obtain stone
Black alkene solution.Graphene dispersing solution being obtained after 2000 leave heart 1h, concentration is measured for 0.60 mg/ml.
Comparative example 1
Weighing 10 mg Graphenes to be dissolved in the 1-Methyl-2-Pyrrolidone of 20 mL, ultrasonic disperse is carried out to which, keeps supersonic frequency
40 kHz of rate, and reaction temperature is kept for 35～45 DEG C, graphene solution is obtained after 5 h, after standing 12h, sedimentation is serious.
Claims (3)
1. a kind of preparation method of graphene dispersing solution, it is characterised in that：Comprise the following steps：
（1）The Graphene of certain mass is dissolved in solvent so as to which concentration is 0.1 ~ 10.0mg/ml, then ball milling mixing, adjusts
Ball milling speed is 100 ~ 500 rpm, and it is 1 that Ball-milling Time is 0 ~ 6 h, ball material volume ratio:3~1:5；
（2）The Graphene liquid of above-mentioned mix homogeneously is carried out decentralized processing using bath ultrasound and mechanical stirring device, is adjusted super
Acoustic frequency is 30 ~ 50 KHz, electric stirring speed is 1000 ~ 10000 rpm, by external circulation cooling system regulation dispersion temperature
Spend for 20-50 DEG C, through the jitter time of 3～20 h, obtain graphene solution；
（3）With the centrifugal speed of 500 ~ 5000rpm, graphene solution is centrifuged, then takes upper solution therein（About
80%）As graphene dispersing solution.
2. the preparation method of a kind of graphene dispersing solution according to claim 1, it is characterised in that：The solvent is 1- first
The mixing of one or more compositions in base -2-Pyrrolidone class, DMF, isopropanol, BDO is molten
Agent.
3. the preparation method of a kind of graphene dispersing solution according to claim 1, it is characterised in that：The Graphene includes
Single-layer graphene, multi-layer graphene and graphene nanometer sheet.
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| CN201610905006.2A CN106430170A (en) | 2016-10-18 | 2016-10-18 | Preparation method of graphene dispersion solution |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107445155A (en) * | 2017-08-10 | 2017-12-08 | 田万鸿 | A kind of graphene dispersing solution and preparation method thereof |
| CN107601478A (en) * | 2017-10-13 | 2018-01-19 | 东北大学 | A kind of preparation method of graphene |
| CN108587572A (en) * | 2018-05-14 | 2018-09-28 | 长沙理工大学 | It is a kind of using ultra-thin graphite slice as the composite phase-change heat-storage material of amorphous matrix and preparation method |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103922323A (en) * | 2014-04-10 | 2014-07-16 | 华侨大学 | Method for preparing small-diameter graphene |
| CN104709903A (en) * | 2015-02-15 | 2015-06-17 | 南京航空航天大学 | Method for preparing few-layer graphene by using auxiliary reagent |
| CN105217612A (en) * | 2015-09-29 | 2016-01-06 | 北京航空航天大学 | A kind of ultrasonic assistant sand mill peels off the method preparing Graphene and the device peeling off Graphene processed |
| CN205419789U (en) * | 2016-03-18 | 2016-08-03 | 绿琪（北京）生物科技有限公司 | Equipment of wet process preparation nanometer graphite alkene |
-
2016
- 2016-10-18 CN CN201610905006.2A patent/CN106430170A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103922323A (en) * | 2014-04-10 | 2014-07-16 | 华侨大学 | Method for preparing small-diameter graphene |
| CN104709903A (en) * | 2015-02-15 | 2015-06-17 | 南京航空航天大学 | Method for preparing few-layer graphene by using auxiliary reagent |
| CN105217612A (en) * | 2015-09-29 | 2016-01-06 | 北京航空航天大学 | A kind of ultrasonic assistant sand mill peels off the method preparing Graphene and the device peeling off Graphene processed |
| CN205419789U (en) * | 2016-03-18 | 2016-08-03 | 绿琪（北京）生物科技有限公司 | Equipment of wet process preparation nanometer graphite alkene |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107445155A (en) * | 2017-08-10 | 2017-12-08 | 田万鸿 | A kind of graphene dispersing solution and preparation method thereof |
| CN107601478A (en) * | 2017-10-13 | 2018-01-19 | 东北大学 | A kind of preparation method of graphene |
| CN108587572A (en) * | 2018-05-14 | 2018-09-28 | 长沙理工大学 | It is a kind of using ultra-thin graphite slice as the composite phase-change heat-storage material of amorphous matrix and preparation method |
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Application publication date: 20170222 |