CN103723712A - Preparation method of single-layer graphene dimethylformamide solution - Google Patents
Preparation method of single-layer graphene dimethylformamide solution Download PDFInfo
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- CN103723712A CN103723712A CN201310591644.8A CN201310591644A CN103723712A CN 103723712 A CN103723712 A CN 103723712A CN 201310591644 A CN201310591644 A CN 201310591644A CN 103723712 A CN103723712 A CN 103723712A
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Abstract
The invention relates to a preparation method of a single-layer graphene dimethylformamide solution. According to the method, graphite is soaked in an intercalator, so that solvent molecules are intercalated into interlayers of the graphite to obtain a graphite intercalation compound, namely, expandable graphite; the expandable graphite is heated quickly under protection of argon, volumes of the solvent molecules on the interlayers of the graphite expand rapidly, the force is larger than Van der Waals' force on the interlayers of the graphite, and then the interlayers of the graphite are expanded out to obtain expanded graphite; after the expanded graphite is obtained, an ultrasonic dispersion liquid-phase stripping method is adopted for stripping screening so as to obtain a graphene solution, and solid graphene powder is obtained after suction filtration, washing and drying; and the solid graphene is ultrasonically dispersed in a dimethylformamide solution, and the graphene dimethylformamide solution which is composited into a membrane material easily with plastic is obtained.
Description
Technical field
The invention belongs to Graphene technical field, be specifically related to a kind of single-layer graphene dimethyl formamide solution preparation method.
Background technology
Graphene, carbon atom is through sp
2the individual layer two dimensional crystal that the mutual bonding of hydridization forms, has the performances such as excellent electricity, calorifics, mechanics, has obtained investigator's extensive concern since 2004 find.It is with a wide range of applications in matrix material, solar cell, sensor field, and be expected to replace silicon materials at semiconductor applications, in various fields such as unicircuit of future generation, energy storage material, flexible display material, bio-pharmaceuticals, aerospace, environment-friendly materials, thermally conductive material, High Strength Steels, having broad application prospects, is impact and the strategic novel material that leads new round Industrial Revolution.
Prior art comprises physical method and chemical process to the preparation method of Graphene, and every kind of method has superiority, and also has shortcoming separately simultaneously.To prepare single crystal graphene film lattice imperfection few for the physical method of graphite to utilize micromechanics to come off, excellent performance, but the method needs the temperature condition of superelevation, and complex process, preparation time is long, and the shortcoming such as yield poorly, is only limited to laboratory fundamental research.Template epitaxial method is under high temperature and uht conditions, in monocrystal SiC surface epitaxy, prepare Graphene, this preparation method can obtain large-area Graphene, but its cost is higher, product is difficult for the promotion and application that from substrate the factor such as separated has greatly limited the method.Limitation based on physical method, chemical process because of its productive rate high, cost is low, the advantage that also can carry out chemically modified to Graphene has caused investigator's concern.The method is under strong acid and strong oxidizer effect, Graphite Powder 99 to be oxidized to intercalation to generate graphite oxide, more ultrasonic peeling off be separated into individual layer and be prepared into the graphene oxide water-sol, finally its deoxidation and reduction is become to Graphene.Wherein, selecting suitable reductive agent is the problem that investigator very pays close attention to.Conventional reductive agent has hydrazine hydrate, Resorcinol, sodium borohydride, reducing sugar, aluminium powder etc., but hydrazine hydrate and Resorcinol have very strong toxicity, harmful to human body and environment; Though xitix is a kind of efficient, environmentally friendly reductive agent, yet it is expensive, be unfavorable for large-scale industrialization production.
Based on existing technology, by N-Methyl pyrrolidone, carry out the graphene aqueous solution that intercalation adds thermal expansion and obtained initial success, but in part industrial use, the aqueous solution does not possess the substance characteristics of other organic compound, cannot meet diversified industrial use.
Summary of the invention
In order to overcome above the deficiencies in the prior art, the invention provides a kind of single-layer graphene dimethyl formamide solution preparation method, utilize N-Methyl pyrrolidone as intercalator, selecting natural graphite is raw material, by repeatedly carrying out the homodisperse single-layer graphene solution of ultrasonic preparation, suction filtration, washing, oven dry obtain Graphene pressed powder, and Graphene solid is dispersed in dimethyl formamide solution through ultrasonic, obtain finely dispersed Graphene dimethyl formamide solution.
The present invention is achieved by the following technical solutions:
A single-layer graphene dimethyl formamide solution preparation method, carries out according to following steps:
(1) configure graphite solution in graphite being joined to organic solution at-5 ~ 0 ℃, fully stir 30min ~ 2h, by the ultrasonic interlayer that makes solvent molecule be intercalation into graphite, obtain expansible black lead;
(2) use argon gas to adequately protect expansible black lead, 80 ~ 90
0in the temperature of C, fully heat 10min ~ 2h, obtain expanded graphite;
(3) utilize the liquid phase stripping method of ultrasonic dispersion to peel off screening to expanded graphite, obtain graphene solution;
(4) pass through again suction filtration, washing, oven dry, obtain Graphene pressed powder;
(5) Graphene solid is dispersed in dimethyl formamide solution through ultrasonic, obtains finely dispersed Graphene dimethyl formamide solution.
Compared with prior art, the invention has the advantages that with N-Methyl pyrrolidone intercalation, adding the product that heat expansion liquid phase stripping method makes can be made into dry powder or be scattered in various dispersion liquids, is conducive to multiple materials such as refinery coke modified activated carbons compound.Graphene is dispersed in dimethyl formamide solution and obtains single-layer graphene dimethyl formamide solution, can improve plastics performance for Graphene-composite plastic film material of a large amount of processability excellences, its Young's modulus and intensity are improved greatly.
Accompanying drawing explanation
Fig. 1 is Graphene atomic force microscope picture.
Fig. 2 is Graphene altitude distribution figure.
Fig. 3 is Graphene scanning electronic microscope schematic diagram.
embodiment:
Below embodiments of the invention are elaborated, the present embodiment is implemented take technical solution of the present invention under prerequisite, provided detailed embodiment and concrete operating process, but protection scope of the present invention is not limited to following embodiment.
Embodiment 1
A single-layer graphene dimethyl formamide solution preparation method, carries out according to following steps:
(1) solution that preparation 100ml is comprised of with the ratio of 1:2 dodecyl triphenyl bromide phosphine and N-Methyl pyrrolidone, in the environment of-3 ℃, the 500 order natural graphite powders of 2g are dipped in solution, and ultrasonic 90min to make solvent molecule be intercalation into graphite intermolecular, obtain expansible black lead.
(2) under argon shield environment, be heated to 85 ℃ and be incubated 30min, obtain expanded graphite.
(3) at operating frequency 60kHZ, under power 160W effect, expanded graphite solution is carried out to ultrasonic peeling off after 90min, obtain black single-layer graphene solution.
(4) graphene solution is carried out to suction filtration, 2% dilute hydrochloric acid washing 2 times for filter cake, deionized water is washed till after neutrality, dries 4h and obtain black Graphene pressed powder in 60 ℃ of baking ovens.
(5) will make Graphene pressed powder is dispersed in 100ml dimethyl formamide solution, at operating frequency 60kHZ, after the lower ultrasonic 1h of power 160W effect, graphene uniform is dispersed in dimethyl formamide solution, obtains black single-layer graphene dimethyl formamide solution.
Embodiment 2
A single-layer graphene dimethyl formamide solution preparation method, carries out according to following steps:
(1) solution that preparation 100ml is comprised of with the ratio of 2:1 dodecyl triphenyl bromide phosphine and N-Methyl pyrrolidone, in the environment of-3 ℃, the 500 order natural graphite powders of 2g are dipped in solution, and ultrasonic 90min to make solvent molecule be intercalation into graphite intermolecular, obtain expansible black lead.
(2) under argon shield environment, be heated to 85 ℃ and be incubated 30min, obtain expanded graphite.
(3) at operating frequency 60kHZ, under power 160W effect, expanded graphite solution is carried out to ultrasonic peeling off after 90min, obtain black single-layer graphene solution.
(4) graphene solution is carried out to suction filtration, 2% dilute hydrochloric acid washing 2 times for filter cake, deionized water is washed till after neutrality, dries 4h and obtain black Graphene pressed powder in 60 ℃ of baking ovens.
(5) will make Graphene pressed powder is dispersed in 100ml dimethyl formamide solution, at operating frequency 60kHZ, after the lower ultrasonic 1h of power 160W effect, graphene uniform is dispersed in dimethyl formamide solution, obtains black single-layer graphene dimethyl formamide solution.
Embodiment 3
A single-layer graphene dimethyl formamide solution preparation method, carries out according to following steps:
(1) get 100ml dodecyl triphenyl bromide phosphine solution, in the environment of-3 ℃, the 500 order natural graphite powders of 2g be dipped in solution, and ultrasonic 90min to make solvent molecule be intercalation into graphite intermolecular, obtain expansible black lead.
(2) under argon shield environment, be heated to 85 ℃ and be incubated 30min, obtain expanded graphite.
(3) at operating frequency 60kHZ, under power 160W effect, expanded graphite solution is carried out to ultrasonic peeling off after 90min, obtain black single-layer graphene solution.
(4) graphene solution is carried out to suction filtration, 2% dilute hydrochloric acid washing 2 times for filter cake, deionized water is washed till after neutrality, dries 4h and obtain black Graphene pressed powder in 60 ℃ of baking ovens.
(5) will make Graphene pressed powder is dispersed in 100ml dimethyl formamide solution, at operating frequency 60kHZ, after the lower ultrasonic 1h of power 160W effect, graphene uniform is dispersed in dimethyl formamide solution, obtains black single-layer graphene dimethyl formamide solution.
Embodiment 4
A single-layer graphene dimethyl formamide solution preparation method, carries out according to following steps:
(1) get 100ml N-Methyl pyrrolidone solution, in the environment of-3 ℃, the 500 order natural graphite powders of 2g be dipped in solution, and ultrasonic 90min to make solvent molecule be intercalation into graphite intermolecular, obtain expansible black lead.
(2) under argon shield environment, be heated to 85 ℃ and be incubated 30min, obtain expanded graphite.
(3) at operating frequency 60kHZ, under power 160W effect, expanded graphite solution is carried out to ultrasonic peeling off after 90min, obtain black single-layer graphene solution.
(4) graphene solution is carried out to suction filtration, 2% dilute hydrochloric acid washing 2 times for filter cake, deionized water is washed till after neutrality, dries 4h and obtain black Graphene pressed powder in 60 ℃ of baking ovens.
(5) will make Graphene pressed powder is dispersed in 100ml dimethyl formamide solution, at operating frequency 60kHZ, after the lower ultrasonic 1h of power 160W effect, graphene uniform is dispersed in dimethyl formamide solution, obtains black single-layer graphene dimethyl formamide solution.
In the preparation process of single-layer graphene dimethyl formamide solution, the effect of selecting N-Methyl pyrrolidone, as intercalator, graphite is peeled off into single-layer graphene is better, and individual layer rate, up to more than 99%, is easy to Graphene and is dispersed in other organic solvents.Finally, utilize shown in atomic power electron microscope Fig. 1-2, and shown in scanning electron microscope diagram 3, the pattern of Graphene and structure are characterized.Shown in atomic force microscope Fig. 1 of Graphene, show that single-layer graphene layer is smooth and level and smooth, shown in thickness chart 2, is about 0.5-1.0nm.Meanwhile, shown in scanning electron microscope diagram sheet Fig. 3 of Graphene, further confirmed the thin layer pattern of Graphene.
Claims (8)
1. a single-layer graphene dimethyl formamide solution preparation method, is characterized in that, according to following steps, carries out:
(1) configure graphite solution in graphite being joined to organic solution at-5 ~ 0 ℃, fully stir 30min ~ 2h, by the ultrasonic interlayer that makes solvent molecule be intercalation into graphite, obtain expansible black lead solution;
(2) use argon gas to adequately protect expansible black lead, 80 ~ 90
0in the temperature of C, fully heat 20min ~ 1h, obtain expanded graphite;
(3) utilize the liquid phase stripping method of ultrasonic dispersion to peel off screening to expanded graphite, obtain graphene solution;
(4) pass through again suction filtration, washing, oven dry, obtain Graphene pressed powder;
(5) Graphene solid is dispersed in dimethyl formamide solution through ultrasonic, obtains finely dispersed Graphene dimethyl formamide solution.
2. single-layer graphene dimethyl formamide solution preparation method according to claim 1, is characterized in that, the organic solution described in step (1) is one or both in dodecyl triphenyl bromide phosphine or N-Methyl pyrrolidone.
3. according to the single-layer graphene dimethyl formamide solution preparation method described in claim l, it is characterized in that, described graphite is 400 ~ 1000 object natural graphite powders.
4. single-layer graphene dimethyl formamide solution preparation method according to claim 1, is characterized in that, the graphite strength of solution described in step (1) is 0.5% ~ 5%.
5. single-layer graphene dimethyl formamide solution preparation method according to claim 1, is characterized in that, ultrasonic described in step (1) is at operating frequency 45kHz, under power 160W effect, and ultrasonic 30min ~ 2h.
6. according to the single-layer graphene dimethyl formamide solution preparation method described in claim l, it is characterized in that, the liquid phase stripping method of the ultrasonic dispersion described in step (3) is at operating frequency 60kHZ, under power 160W effect, existing expanded graphite solution is carried out to the ultrasonic 30min ~ 2h that peels off.
7. according to the single-layer graphene dimethyl formamide solution preparation method described in claim l, it is characterized in that, suction filtration described in step (4), washing, oven dry are for to carry out suction filtration by graphene solution, 2% dilute hydrochloric acid washing 1 ~ 5 time for the filter cake obtaining, the filter cake of suction filtration is extremely neutral with deionized water wash again, after suction filtration, in 60 ℃ of baking ovens, dry 2 ~ 12h.
8. according to the single-layer graphene dimethyl formamide solution preparation method described in claim l, it is characterized in that, Graphene solid is dispersed in dimethyl formamide solution as the single-layer graphene solid obtaining is added in solvent dimethylformamide through ultrasonic described in step (5), at operating frequency 60kHZ, the lower ultrasonic 30min ~ 2h of power 160W effect, is dispersed in dimethyl formamide solution graphene uniform.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103922325A (en) * | 2014-04-17 | 2014-07-16 | 哈尔滨工程大学 | Graphene preparation method |
| CN106517173A (en) * | 2016-10-28 | 2017-03-22 | 蚌埠玻璃工业设计研究院 | Preparation method of graphene dispersion liquid |
| CN106829937A (en) * | 2017-01-16 | 2017-06-13 | 王奉瑾 | A kind of preparation method of Graphene |
| CN108899534A (en) * | 2018-06-19 | 2018-11-27 | 清华大学 | A kind of preparation method of lithium ion battery capacitor positive electrode vanadium oxide |
| CN113772732A (en) * | 2021-09-26 | 2021-12-10 | 江南大学 | Method for preparing two-dimensional material nanosheet by DEET stripping |
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| CN102659096A (en) * | 2012-04-27 | 2012-09-12 | 湖南大学 | Preparation methods of graphene dispersion solution and thin film of graphene |
| CN103213979A (en) * | 2013-05-10 | 2013-07-24 | 山西大同大学 | Method for preparing graphene by solvent-thermal process |
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| CN102659096A (en) * | 2012-04-27 | 2012-09-12 | 湖南大学 | Preparation methods of graphene dispersion solution and thin film of graphene |
| CN103213979A (en) * | 2013-05-10 | 2013-07-24 | 山西大同大学 | Method for preparing graphene by solvent-thermal process |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103922325A (en) * | 2014-04-17 | 2014-07-16 | 哈尔滨工程大学 | Graphene preparation method |
| CN103922325B (en) * | 2014-04-17 | 2015-12-09 | 哈尔滨工程大学 | A kind of preparation method of Graphene |
| CN106517173A (en) * | 2016-10-28 | 2017-03-22 | 蚌埠玻璃工业设计研究院 | Preparation method of graphene dispersion liquid |
| CN106829937A (en) * | 2017-01-16 | 2017-06-13 | 王奉瑾 | A kind of preparation method of Graphene |
| CN106829937B (en) * | 2017-01-16 | 2019-03-22 | 王奉瑾 | A kind of preparation method of graphene |
| CN108899534A (en) * | 2018-06-19 | 2018-11-27 | 清华大学 | A kind of preparation method of lithium ion battery capacitor positive electrode vanadium oxide |
| CN108899534B (en) * | 2018-06-19 | 2021-03-16 | 清华大学 | Preparation method of vanadium oxide as positive electrode material of lithium ion battery capacitor |
| CN113772732A (en) * | 2021-09-26 | 2021-12-10 | 江南大学 | Method for preparing two-dimensional material nanosheet by DEET stripping |
| CN113772732B (en) * | 2021-09-26 | 2022-05-06 | 江南大学 | Method for preparing two-dimensional material nanosheet by DEET stripping |
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