CN103738949A - Preparation method for single-layer graphene isopropanol solution - Google Patents
Preparation method for single-layer graphene isopropanol solution Download PDFInfo
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- CN103738949A CN103738949A CN201310592856.8A CN201310592856A CN103738949A CN 103738949 A CN103738949 A CN 103738949A CN 201310592856 A CN201310592856 A CN 201310592856A CN 103738949 A CN103738949 A CN 103738949A
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Abstract
The invention relates to a preparation method for a single-layer graphene isopropanol solution. The method includes: soaking graphite into an intercalation agent to make solvent molecules intercalated into interlayers of graphite so as to obtain a graphite intercalation compound, i.e. expansible graphite; then heating the expansible graphite rapidly under argon protection to make the solvent molecular in the interlayers of graphite largen and expand quickly in volume, letting the force greater than the Van der Waals' force between graphite layers expand the graphite layers, thus obtaining expanded graphite; then carrying out stripping screening by an ultrasonic dispersion liquid phase stripping technique to obtain a graphene solution, and then carrying out pumping filtering, washing and drying to obtain graphene solid powder; subjecting the graphene solids to ultrasonic dispersion in an isopropanol solution, thus obtaining the graphene isopropanol solution that has important application in preparation of graphene high polymer masterbatches.
Description
Technical field
The invention belongs to Graphene technical field, be specifically related to a kind of single-layer graphene aqueous isopropanol preparation method.
Background technology
Graphene is a kind of two dimensional crystal of the carbon atom individual layer that is honeycomb fashion hexagonal array, there is excellent electricity, calorifics and mechanical property, 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, 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 the promotion and application that its cost is higher, product is difficult for greatly having limited from factors such as substrate separate the method.Based on the limitation of 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, but 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 aqueous isopropanol 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 aqueous isopropanol through ultrasonic, obtain finely dispersed Graphene aqueous isopropanol.
The present invention is achieved by the following technical solutions:
A kind of single-layer graphene aqueous isopropanol 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, 70 ~ 80
0in the temperature of C, fully heat 30min ~ 4h, 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 aqueous isopropanol through ultrasonic, obtains finely dispersed Graphene aqueous isopropanol.
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.Virahol is as the dispersion agent of Graphene, has important use preparing Graphene polymer master batch.
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 under take technical solution of the present invention as prerequisite, provided detailed embodiment and concrete operating process, but protection scope of the present invention is not limited to following embodiment.
Embodiment 1
A kind of single-layer graphene aqueous isopropanol 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 4.5g 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 78 ℃ and be incubated 1h, 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 and be dispersed in 100ml aqueous isopropanol, and at operating frequency 60kHZ, after the lower ultrasonic 1h of power 160W effect, graphene uniform will be dispersed in aqueous isopropanol, obtain black single-layer graphene aqueous isopropanol.
Embodiment 2
A kind of single-layer graphene aqueous isopropanol 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 4.5g 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 78 ℃ and be incubated 1h, 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 and be dispersed in 100ml aqueous isopropanol, and at operating frequency 60kHZ, after the lower ultrasonic 1h of power 160W effect, graphene uniform will be dispersed in aqueous isopropanol, obtain black single-layer graphene aqueous isopropanol.
Embodiment 3
A kind of single-layer graphene aqueous isopropanol 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 4.5g 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 78 ℃ and be incubated 1h, 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 and be dispersed in 100ml aqueous isopropanol, and at operating frequency 60kHZ, after the lower ultrasonic 1h of power 160W effect, graphene uniform will be dispersed in aqueous isopropanol, obtain black single-layer graphene aqueous isopropanol.
Embodiment 4
A kind of single-layer graphene aqueous isopropanol 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 4.5g 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 78 ℃ and be incubated 1h, 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 and be dispersed in 100ml aqueous isopropanol, and at operating frequency 60kHZ, after the lower ultrasonic 1h of power 160W effect, graphene uniform will be dispersed in aqueous isopropanol, obtain black single-layer graphene aqueous isopropanol.
In the preparation process of single-layer graphene aqueous isopropanol, 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, pattern and structure to Graphene characterize.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 aqueous isopropanol 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, 70 ~ 80
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 aqueous isopropanol through ultrasonic, obtains finely dispersed Graphene aqueous isopropanol.
2. single-layer graphene aqueous isopropanol 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 aqueous isopropanol preparation method described in claim l, it is characterized in that, described graphite is 400 ~ 1000 object natural graphite powders.
4. single-layer graphene aqueous isopropanol preparation method according to claim 1, is characterized in that, the graphite strength of solution described in step (1) is 1% ~ 5%.
5. single-layer graphene aqueous isopropanol 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 aqueous isopropanol 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 aqueous isopropanol 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 aqueous isopropanol preparation method described in claim l, it is characterized in that, Graphene solid is dispersed in aqueous isopropanol as the single-layer graphene solid obtaining is added in isopropanol solvent through ultrasonic described in step (5), at operating frequency 60kHZ, the lower ultrasonic 30min ~ 2h of power 160W effect, is dispersed in aqueous isopropanol graphene uniform.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104556020A (en) * | 2015-01-23 | 2015-04-29 | 青岛科技大学 | Preparation method of graphene ethanol dispersion solution |
| CN106744886A (en) * | 2017-01-16 | 2017-05-31 | 王奉瑾 | A kind of method that Graphene is prepared based on purification by liquid extraction technology |
| CN106744885A (en) * | 2017-01-16 | 2017-05-31 | 王奉瑾 | A kind of device for preparing Graphene |
| CN106829937A (en) * | 2017-01-16 | 2017-06-13 | 王奉瑾 | A kind of preparation method of Graphene |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102115078A (en) * | 2011-01-19 | 2011-07-06 | 上海交通大学 | Method for preparing graphene by using supercritical fluid |
| CN102659096A (en) * | 2012-04-27 | 2012-09-12 | 湖南大学 | Preparation methods of graphene dispersion solution and thin film of graphene |
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- 2013-11-22 CN CN201310592856.8A patent/CN103738949A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102115078A (en) * | 2011-01-19 | 2011-07-06 | 上海交通大学 | Method for preparing graphene by using supercritical fluid |
| CN102659096A (en) * | 2012-04-27 | 2012-09-12 | 湖南大学 | Preparation methods of graphene dispersion solution and thin film of graphene |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104556020A (en) * | 2015-01-23 | 2015-04-29 | 青岛科技大学 | Preparation method of graphene ethanol dispersion solution |
| CN106744886A (en) * | 2017-01-16 | 2017-05-31 | 王奉瑾 | A kind of method that Graphene is prepared based on purification by liquid extraction technology |
| CN106744885A (en) * | 2017-01-16 | 2017-05-31 | 王奉瑾 | A kind of device for preparing Graphene |
| CN106829937A (en) * | 2017-01-16 | 2017-06-13 | 王奉瑾 | A kind of preparation method of Graphene |
| CN106744886B (en) * | 2017-01-16 | 2019-02-26 | 王奉瑾 | A method of graphene is prepared based on purification by liquid extraction technology |
| CN106744885B (en) * | 2017-01-16 | 2019-03-01 | 王奉瑾 | A kind of device being used to prepare graphene |
| CN106829937B (en) * | 2017-01-16 | 2019-03-22 | 王奉瑾 | A kind of preparation method of graphene |
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