CN105836737A - Method for preparing graphene by combining ultrasonic peeling and jet flow peeling - Google Patents
Method for preparing graphene by combining ultrasonic peeling and jet flow peeling Download PDFInfo
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- CN105836737A CN105836737A CN201610296912.7A CN201610296912A CN105836737A CN 105836737 A CN105836737 A CN 105836737A CN 201610296912 A CN201610296912 A CN 201610296912A CN 105836737 A CN105836737 A CN 105836737A
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Abstract
The invention discloses a method for preparing graphene by combining ultrasonic peeling and jet flow peeling. The method comprises the steps that firstly, graphite is dispersed in an aqueous surfactant solution; secondly, the mixed liquid obtained in the first step is subjected to ultrasonic peeling, and multilayer graphene dispersion liquid is obtained; thirdly, the multilayer graphene dispersion liquid obtained in the second step is subjected to jet flow peeling, and monolayer graphene dispersion liquid is obtained; fourthly, the monolayer graphene dispersion liquid obtained in the third step is dried, and the graphene is obtained. According to the preparation method, the ultrasound and jet flow combined peeling mode is adopted for the first time, the obtained graphene in the dispersion liquid has few structural defects and layers and high concentration, the excellent performance of graphene is retained very well, and the graphene can be widely applied to the fields of automotive parts, sensors, conductive materials, heat conduction materials and the like. The method is economical and environmentally friendly, the raw material utilization rate is increased, and the industrialization cost is reduced.
Description
Technical field
The invention belongs to Graphene functional material preparing technical field, be specifically related to the ultrasonic stripping of a kind of employing and tie mutually with jet stripping
The method of Graphene is prepared in conjunction.
Technical background
Since Graphene was prepared in 2004 in peace moral strong K sea nurse (Andre K.Geim) etc. of Univ Manchester UK
Material, owing to structure and the photoelectric property of its uniqueness receive people and pay attention to widely.Graphene is made up of one layer of carbon atom
Two-dimensional Carbon nano material, is to be currently known the thinnest two-dimensional material, and thickness is only 0.34nm.Mono-layer graphite is due to its big ratio table
Area, excellent conduction, heat conductivility and low thermal coefficient of expansion and be considered as preferable material.Can macromolecular material,
It is used widely in the fields such as ultracapacitor, fiber, electrode material, electronics.
At present the preparation method of Graphene have mechanical stripping method, ultrahigh vacuum Graphene epitaxial growth method, chemical vapour deposition technique,
Oxidation-reduction method, electrolysis, ultrasonic stripping method, solvent-thermal method etc..The Graphene quality that wherein prepared by mechanical stripping method is the highest,
But its yield is the lowest, is only used for scientific research；The high cost of ultrahigh vacuum Graphene epitaxial growth method and the knot of sequin
Structure limits its application；Chemical gaseous phase deposition is few with Graphene defect prepared by epitaxial growth method, but high to equipment requirement, former
Material conversion ratio is low, significantly limit its application；Although oxidation-reduction method prepares Graphene can the less stone of the large-scale production number of plies
Ink alkene, but the destruction of Graphene lattice is made its hexagonal honeycomb crystal structure to restore by strong oxidizer, causes its partial properties
Disappearance；Electrolysis can synthesize substantial amounts of Graphene, but the surface of the Graphene synthesized all with substantial amounts of cation or bear from
Son or organic matter；Ultrasonic stripping method is with graphite or expanded graphite as raw material, and equipment requirement is low, and energy consumption is low, and the Graphene of preparation
Defect is few, and concentration is high it is considered to be the most promising preparation method of one；The Graphene purity of hot solvent method synthesis is higher, but
It is that the reaction time is relatively long, and productivity only has 1～5%.
Summary of the invention
It is an object of the invention to overcome the deficiencies in the prior art, it is provided that the ultrasonic stripping of a kind of employing peels off, with jet, the preparation that combines
The method of Graphene.The preparation method of the present invention uses the ultrasonic stripping mode combined with jet, the dispersion prepared first
In liquid, graphene-structured defect is few, and the number of plies is few, and concentration is high, and remains the excellent properties of Graphene well, can extensively apply
In fields such as auto parts and components, sensor, conductive material, Heat Conduction Materials.The inventive method is economic and environment-friendly, has both improved raw material profit
By rate, reduce again industrialization cost.
The purpose of the present invention is achieved through the following technical solutions:
It is an object of the invention to provide and a kind of use ultrasonic stripping and jet to peel off the method preparing Graphene that combines, including:
(1) by graphite dispersion in aqueous surfactant solution；
(2) mixed liquor that step (1) obtains is carried out ultrasonic stripping, obtain graphene dispersing solution I, i.e. multi-layer graphene and divide
Dissipate liquid；
(3) graphene dispersing solution I (multi-layer graphene dispersion liquid) step (2) obtained carries out jet stripping, obtains stone
Ink alkene dispersion liquid II, i.e. single-layer graphene dispersion liquid；
(4) graphene dispersing solution II (single-layer graphene dispersion liquid) step (3) obtained is dried process, prepares stone
Ink alkene product.
Further, in described step (1), the purity of graphite is 99.90wt%～99.95wt%, median particle diameter (D50) be 10～
100μm。
Further, in described step (1) surfactant be selected from neopelex, cetyl trimethylammonium bromide,
One or more in lauryl sodium sulfate, sodium lignin sulfonate.
Further, in described step (1), the mass concentration of aqueous surfactant solution is 0.5～5.0g/L.
Further, in described step (1), the mass concentration of graphite is 25～75g/L.
Further, in described step (2), the power of ultrasonic stripping is 300～1000W, and the time is 6～12 hours.
Further, the mass concentration of Graphene in graphene dispersing solution I (multi-layer graphene dispersion liquid) in described step (2)
It is 25～75g/L.
Further, the flow velocity that in described step (3), jet is peeled off is 300～400L/h, and feed pump pressure 2～4bar goes out
Material temperature degree ＜ 60 DEG C, nozzle exit pressure 300～1000bar, cycle-index 4～8 times.
Further, in described step (4), vacuum drying temperature is 80～100 DEG C, and the time is 3～6 hours.
Compared with prior art, the positive effect of the present invention is as follows:
The preparation method cost of the present invention is relatively low, purity and the preparation method of the higher Graphene of productivity.Have an advantage in that:
(1) preparation method of the present invention uses graphite as raw material, low price low cost, is relatively easily peeled into Graphene, and
And it is greatly improved productivity；
(2) water and surfactant is used to peel off reagent, safer, environmental protection and environmental friendliness as intercalation；
(3) preparation method is simple to equipment requirement, easy to operate, and production stage is few, is suitable for large-scale production.
(4) the graphene-structured defect using the preparation method of the present invention to obtain is few, and the number of plies is few, and concentration is high, and retains well
The excellent properties of Graphene.
Accompanying drawing explanation
Fig. 1 is ultrasonic stripping off device schematic diagram.
Fig. 2 is jet stripping off device schematic diagram.
Fig. 3 is single ultrasonic lift-off processing technique TEM collection of illustrative plates.
Fig. 4 is single jet lift-off processing technique TEM collection of illustrative plates.
Fig. 5 is the TEM collection of illustrative plates of the Graphene of embodiment 5 preparation.
Fig. 6 is the XRD analysis of spectrum of the black alkene of embodiment 5 preparation.
Detailed description of the invention
Below in conjunction with embodiment and accompanying drawing, the present invention is described in further detail, but embodiments of the present invention are not limited to this.
Fig. 1 is ultrasonic stripping off device schematic diagram, is delivered in ultrasonic device by peristaltic pump by the material in mixing plant, passes through
Being back in mixing plant after ultrasonic stripping, by circulation until getting a desired effect, in this technological process, major control is ultrasonic
The power of equipment and ultrasonic time；
Fig. 2 is jet stripping off device schematic diagram, and material is delivered at nozzle through membrane pump, and at nozzle, after high-pressure, jet is extremely
In cavity, after cavity filtration under diminished pressure, output is back to charging basket, major control flow velocity, feed pump pressure in this technological process, goes out
Material mouth temperature, nozzle exit pressure and cycle-index.
Graphite raw material in following example is bought from tsingtauite sea material with carbon element Co., Ltd.
Embodiment 1
1, preparation 0.5g/L sodium dodecyl benzene sulfonate aqueous solution, high-speed stirred 30 minutes；
2, being 99.90wt% by purity, median particle diameter (D50) is the neopelex that the graphite of 10 μm joins step 1
In the aqueous solution, graphite concentration is 25g/L, high-speed stirred 30 minutes；
3, carrying out ultrasonic stripping by Fig. 1 ultrasonic stripping off device schematic diagram, wherein ultrasonic power is 300W, and ultrasonic time is 12 hours；
4, carrying out jet stripping by Fig. 2 jet stripping off device schematic diagram, wherein flow velocity is 300L/h, and feed pump pressure is 2bar, goes out
Material mouth temperature is 56 DEG C, and nozzle exit pressure is 300bar, and cycle-index is 8 times；
5, vacuum drying obtains Graphene, and wherein baking temperature is 80 DEG C, and drying time is 6h.
Embodiment 2
1, the preparation 1.0g/L cetyl trimethylammonium bromide aqueous solution, high-speed stirred 30 minutes；
2, being 99.90wt% by purity, median particle diameter (D50) is the cetyl trimethyl bromine that the graphite of 60 μm joins step 1
Changing in aqueous ammonium, graphite concentration is 50g/L, high-speed stirred 30 minutes；
3, carrying out ultrasonic stripping by Fig. 1 ultrasonic stripping off device schematic diagram, wherein ultrasonic power is 500W, and ultrasonic time is 10 hours；
4, carrying out jet stripping by Fig. 2 jet stripping off device schematic diagram, wherein flow velocity is 350L/h, and feed pump pressure is 3bar, goes out
Material mouth temperature is 58 DEG C, and nozzle exit pressure is 500bar, and cycle-index is 7 times；
5, vacuum drying obtains Graphene, and wherein baking temperature is 80 DEG C, and drying time is 6h.
Embodiment 3
1, preparation 2.0g/L lauryl sodium sulfate aqueous solution, high-speed stirred 30 minutes；
2, being 99.95wt% by purity, median particle diameter (D50) is the lauryl sodium sulfate water that the graphite of 50 μm joins step 1
In solution, graphite concentration is 50g/L, high-speed stirred 30 minutes；
3, carrying out ultrasonic stripping by Fig. 1 ultrasonic stripping off device schematic diagram, wherein ultrasonic power is 750W, and ultrasonic time is 8 hours；
4, carrying out jet stripping by Fig. 2 jet stripping off device schematic diagram, wherein flow velocity is 350L/h, and feed pump pressure is 3bar, goes out
Material mouth temperature is 57 DEG C, and nozzle exit pressure is 700bar, and cycle-index is 5 times；
5, vacuum drying obtains Graphene, and wherein baking temperature is 80 DEG C, and drying time is 5h.
Embodiment 4
1, preparation 3.0g/L lignin sulfonic acid sodium water solution, high-speed stirred 30 minutes；
2, being 99.95wt% by purity, it is water-soluble that median particle diameter (D50) is that the graphite of 80 μm joins the sodium lignin sulfonate of step 1
In liquid, graphite concentration is 75g/L, high-speed stirred 30 minutes；
3, carrying out ultrasonic stripping by Fig. 1 ultrasonic stripping off device schematic diagram, wherein ultrasonic power is 800W, and ultrasonic time is 6 hours；
4, carrying out jet stripping by Fig. 2 jet stripping off device schematic diagram, wherein flow velocity is 400L/h, and feed pump pressure is 4bar, goes out
Material mouth temperature is 55 DEG C, and nozzle exit pressure is 1000bar, and cycle-index is 8 times；
5, vacuum drying obtains Graphene, and wherein baking temperature is 100 DEG C, and drying time is 3h.
Embodiment 5
1, preparation 5.0g/L neopelex and cetyl trimethylammonium bromide mixed aqueous solution (neopelex
It is 1:1 with cetyl trimethylammonium bromide mass ratio), high-speed stirred 30 minutes；
2, being 99.95wt% by purity, median particle diameter (D50) is in the mixed aqueous solution that the graphite of 100 μm joins step 1,
Graphite concentration is 75g/L, high-speed stirred 30 minutes；
3, carrying out ultrasonic stripping by Fig. 1 ultrasonic stripping off device schematic diagram, wherein ultrasonic power is 1000W, and ultrasonic time is 10 hours；
4, carrying out jet stripping by Fig. 2 jet stripping off device schematic diagram, wherein flow velocity is 400L/h, and feed pump pressure is 4bar, goes out
Material mouth temperature is 56 DEG C, and nozzle exit pressure is 1000bar, and cycle-index is 6 times；
5, vacuum drying obtains Graphene, and wherein baking temperature is 100 DEG C, and drying time is 4h.
Comparative example 1
1, preparation 5.0g/L neopelex and cetyl trimethylammonium bromide mixed aqueous solution (neopelex
It is 1:1 with cetyl trimethylammonium bromide mass ratio), high-speed stirred 30 minutes；
2, being 99.95wt% by purity, median particle diameter (D50) is in the mixed aqueous solution that the graphite of 100 μm joins step 1,
Graphite quality concentration is 75g/L, high-speed stirred 30 minutes；
3, carrying out ultrasonic stripping by Fig. 1 ultrasonic stripping off device schematic diagram, wherein ultrasonic power is 1000W, and ultrasonic time is 10 hours；
4, vacuum drying obtains Graphene, and wherein baking temperature is 100 DEG C, and drying time is 4h.
Comparative example 2
1, preparation 5.0g/L neopelex and cetyl trimethylammonium bromide mixed aqueous solution (neopelex
It is 1:1 with cetyl trimethylammonium bromide mass ratio), high-speed stirred 30 minutes；
2, being 99.95wt% by purity, median particle diameter (D50) is in the mixed aqueous solution that the graphite of 100 μm joins step 1,
Graphite quality concentration is 75g/L, high-speed stirred 30 minutes；
3, carrying out jet stripping by Fig. 2 jet stripping off device schematic diagram, wherein flow velocity is 400L/h, and feed pump pressure is 4bar, goes out
Material mouth temperature is 56 DEG C, and nozzle exit pressure is 1000bar, and cycle-index is 6 times；
4, vacuum drying obtains Graphene, and wherein baking temperature is 100 DEG C, and drying time is 4h.
Refer to Fig. 5 and Fig. 6, show Graphene TEM collection of illustrative plates and the XRD analysis of spectrum of embodiment 5 preparation.Compare contrast
Example 1 uses the Graphene TEM (such as Fig. 3) of single ultrasonic lift-off processing and comparative example 2 to use the graphite of single jet lift-off processing
Alkene TEM (such as Fig. 4), it can be seen that embodiment 5 can obtain the Graphene product that purity is higher, and this Graphene product has
Good laminated structure.
Claims (9)
1. use ultrasonic stripping to peel off, with jet, the method preparing Graphene that combines, including:
(1) by graphite dispersion in aqueous surfactant solution；
(2) mixed liquor that step (1) obtains is carried out ultrasonic stripping, obtain graphene dispersing solution I；
(3) graphene dispersing solution I that step (2) obtains is carried out jet stripping, obtain graphene dispersing solution II；
(4) graphene dispersing solution II that step (3) obtains is dried process, prepares Graphene.
The most according to claim 1 a kind of using ultrasonic stripping and jet to peel off the method preparing Graphene that combines, it is special
Levying and be: in described step (1), the purity of graphite is 99.90wt%～99.95wt%, median particle diameter D50 is 10～100 μm.
The most according to claim 1 a kind of using ultrasonic stripping and jet to peel off the method preparing Graphene that combines, it is special
Levy and be: in described step (1), surfactant is selected from neopelex, cetyl trimethylammonium bromide, 12
One or more in sodium alkyl sulfate, sodium lignin sulfonate.
The most according to claim 1 a kind of using ultrasonic stripping and jet to peel off the method preparing Graphene that combines, it is special
Levy and be: in described step (1), the mass concentration of aqueous surfactant solution is 0.5～5.0g/L.
The most according to claim 1 a kind of using ultrasonic stripping and jet to peel off the method preparing Graphene that combines, it is special
Levy and be: in described step (1), the mass concentration of graphite is 25～75g/L.
The most according to claim 1 a kind of using ultrasonic stripping and jet to peel off the method preparing Graphene that combines, it is special
Levying and be: in described step (2), the power of ultrasonic stripping is 300～1000W, the time is 6～12 hours.
The most according to claim 1 a kind of using ultrasonic stripping and jet to peel off the method preparing Graphene that combines, it is special
Levy and be: in the graphene dispersing solution I in described step (2), the mass concentration of Graphene is 25～75g/L.
The most according to claim 1 a kind of using ultrasonic stripping and jet to peel off the method preparing Graphene that combines, it is special
Levy and be: the flow velocity that in described step (3), jet is peeled off is 300～400L/h, feed pump pressure 2～4bar, drop temperature
＜ 60 DEG C, nozzle exit pressure 300～1000bar, cycle-index 4～8 times.
The most according to claim 1 a kind of using ultrasonic stripping and jet to peel off the method preparing Graphene that combines, it is special
Levy and be: in described step (4), vacuum drying temperature is 80～100 DEG C, and the time is 3～6 hours.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106219535A (en) * | 2016-08-16 | 2016-12-14 | 南京工业大学 | A kind of scale continuous high-efficient peels off the method for graphite oxide |
| CN107161993A (en) * | 2017-07-03 | 2017-09-15 | 北京旭碳新材料科技有限公司 | High concentration graphene slurry and preparation method thereof and device |
| TWI668187B (en) * | 2016-10-07 | 2019-08-11 | 林逸樵 | Device for rapidly producing graphene and method thereof |
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| CN102701190A (en) * | 2012-05-31 | 2012-10-03 | 格雷菲尼（北京）科技有限公司 | Process and method for preparing graphene in mixed solution of water and acetone |
| CN103977870A (en) * | 2014-05-26 | 2014-08-13 | 北京航空航天大学 | Process and device for preparing graphene precursor two-dimension nanoscale graphite powder by adopting airflow crushing and peeling method |
| JP5688669B1 (en) * | 2014-09-09 | 2015-03-25 | グラフェンプラットフォーム株式会社 | Graphite-based carbon material used as graphene precursor, graphene dispersion containing the same, graphene composite, and method for producing the same |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102583332A (en) * | 2012-01-17 | 2012-07-18 | 北京航空航天大学 | Technology and method for preparing solution used for preparing graphene in liquid phase |
| CN102701190A (en) * | 2012-05-31 | 2012-10-03 | 格雷菲尼（北京）科技有限公司 | Process and method for preparing graphene in mixed solution of water and acetone |
| CN103977870A (en) * | 2014-05-26 | 2014-08-13 | 北京航空航天大学 | Process and device for preparing graphene precursor two-dimension nanoscale graphite powder by adopting airflow crushing and peeling method |
| JP5688669B1 (en) * | 2014-09-09 | 2015-03-25 | グラフェンプラットフォーム株式会社 | Graphite-based carbon material used as graphene precursor, graphene dispersion containing the same, graphene composite, and method for producing the same |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106219535A (en) * | 2016-08-16 | 2016-12-14 | 南京工业大学 | A kind of scale continuous high-efficient peels off the method for graphite oxide |
| TWI668187B (en) * | 2016-10-07 | 2019-08-11 | 林逸樵 | Device for rapidly producing graphene and method thereof |
| CN107161993A (en) * | 2017-07-03 | 2017-09-15 | 北京旭碳新材料科技有限公司 | High concentration graphene slurry and preparation method thereof and device |
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Application publication date: 20160810 Assignee: Shanghai Li Sheng Nano Technology Co., Ltd. Assignor: Shanghai Co., Ltd of Li Wusheng enterprise group Contract record no.: X2019310000016 Denomination of invention: Method for preparing graphene by combining ultrasonic peeling and jet flow peeling Granted publication date: 20181109 License type: Exclusive License Record date: 20191015 |