CN103723708A - Preparation method of organic single-layer graphene solution - Google Patents
Preparation method of organic single-layer graphene solution Download PDFInfo
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- CN103723708A CN103723708A CN201310591123.2A CN201310591123A CN103723708A CN 103723708 A CN103723708 A CN 103723708A CN 201310591123 A CN201310591123 A CN 201310591123A CN 103723708 A CN103723708 A CN 103723708A
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Abstract
The invention relates to a preparation method of an organic single-layer graphene 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, and expanded graphite is obtained; 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 an organic solution, and the organic graphene solution which is high in single layer rate and uniform in dispersion and has corrosion inhibition on a metal composite is obtained finally.
Description
Technical field
The invention belongs to Graphene technical field, be specifically related to a kind of single-layer graphene organic solution preparation method.
Background technology
Graphene, carbon atom is through sp
2the individual layer two dimensional crystal of the mutual bonding composition of hydridization, it is the basic structural unit that builds other dimension carbon materials (zero dimension soccerballene, one dimension carbon nanotube, three-dimensional graphite).Due to its excellent electricity, calorifics and mechanical property, be expected to obtain widespread use in fields such as high function nanometer electronic device, nesa coating, matrix material, catalytic material, energy storage materials, therefore from the study group of Univ Manchester UK in 2004, obtain first after the Graphene of stable existence, it just obtains the extensive concern of studying.Graphene has broad application prospects 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, is impact and the strategic novel material that leads new round Industrial Revolution.Therefore urgently seek a kind of method of preparing in a large number Graphene.
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, and needs the temperature condition of superelevation, complex process, and 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 acquired preliminary success of graphene aqueous solution preparation method that intercalation adds thermal expansion, 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 organic solution preparation method, utilize N-Methyl pyrrolidone or dodecyl triphenyl bromide phosphine 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 organic solution through ultrasonic, obtain finely dispersed Graphene organic solution.
The present invention is achieved by the following technical solutions:
A kind of single-layer graphene organic solution preparation method, carries out according to following steps:
(1) prepare graphite solution in graphite being joined to organic solvent at-10 ~ 0 ℃, fully stir 30min ~ 2h, by the ultrasonic interlayer that makes solvent molecule be intercalation into graphite, obtain expansible black lead solution;
(2), under argon shield atmosphere, expansible black lead solution is heated to 80 ~ 100
0c, insulation 20min ~ 1h, obtains 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 pressed powder is dispersed in organic solvent through ultrasonic, obtains finely dispersed Graphene organic solution.
Described single-layer graphene organic solution preparation method, the organic solvent described in step (1) can be one or both mixtures in dodecyl triphenyl bromide phosphine or N-Methyl pyrrolidone.
Described single-layer graphene organic solution preparation method, the graphite described in step (1) is can 400 ~ 1000 object natural graphite powders.
Described single-layer graphene organic solution preparation method, the graphite concentration of polymer solution described in step (1) can be 0.5% ~ 5%.
Described single-layer graphene organic solution preparation method, ultrasonic described in step (1) can be at operating frequency 45kHz, under power 160W effect, ultrasonic 30min ~ 2h.
Described single-layer graphene organic solution preparation method, the liquid phase stripping method parameter of the ultrasonic dispersion described in step (3) can be: operating frequency 60kHZ, power 160W, ultrasonic splitting time 30min ~ 2h.
Described single-layer graphene organic solution preparation method, suction filtration described in step (4), washing, oven dry can be for to carry out suction filtration by graphene solution, the filter cake obtaining fully washs with mass concentration 2% dilute hydrochloric acid, 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.
Described single-layer graphene organic solution preparation method, the parameter of the ultrasonic dispersion described in step (5) can be: at operating frequency 60kHZ, power 160W, ultrasonication time 30min ~ 2h.
Described single-layer graphene organic solution preparation method, the organic solvent described in step (5) can be the one in pyridine, dimethyl formamide, dimethyl sulfoxide (DMSO), toluene, ethylene glycol, Virahol or propyl carbinol.
Compared with prior art, the invention has the advantages that the effect of graphite being peeled off into single-layer graphene with N-Methyl pyrrolidone or dodecyl triphenyl bromide phosphine is better, individual layer rate is up to more than 99%, the product making 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 and in organic solution, obtains single-layer graphene organic solution, can be widely used in the industrial uses such as ultracapacitor, lithium cell, sensor, synthetic rubber, modified plastics, organometallic compound, anion-exchange membrane, and Graphene-metal composite is had to corrosion inhibition.
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 organic 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-5 ℃, the 400 order natural graphite powders of 1g are dipped in solution, fully stir 30min, at operating frequency 45kHz, under power 160W effect, it is intermolecular that ultrasonic 50min makes solvent molecule be intercalation into graphite, obtains expansible black lead.
(2) under argon shield environment, be heated to 80 ℃ and be incubated 20min, obtain expanded graphite.
(3) at operating frequency 60kHZ, under power 160W effect, expanded graphite solution is carried out to ultrasonic peeling off after 50min, 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 pyridine, and at operating frequency 60kHZ, after the lower ultrasonic 1h of power 160W effect, graphene uniform will be dispersed in pyridine, obtain black single-layer graphene pyridine solution.
Embodiment 2
A kind of single-layer graphene organic 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-8 ℃, the 600 order natural graphite powders of 5g are dipped in solution, fully stir 70min, at operating frequency 45kHz, under power 160W effect, it is intermolecular that ultrasonic 2h makes solvent molecule be intercalation into graphite, obtains expansible black lead.
(2) under argon shield environment, be heated to 100 ℃ and be incubated 50min, obtain expanded graphite.
(3) at operating frequency 60kHZ, under power 160W effect, expanded graphite solution is carried out to ultrasonic peeling off after 2h, obtain black single-layer graphene solution.
(4) graphene solution is carried out to suction filtration, 2% dilute hydrochloric acid washing 5 times for filter cake, deionized water is washed till after neutrality, dries 12h and obtain black Graphene pressed powder in 60 ℃ of baking ovens.
(5) will make Graphene pressed powder and be dispersed in 100ml dimethyl formamide, and at operating frequency 60kHZ, after the lower ultrasonic 2h of power 160W effect, graphene uniform will be dispersed in dimethyl formamide, obtain black single-layer graphene dimethyl formamide solution.
Embodiment 3
A kind of single-layer graphene organic solution preparation method, carries out according to following steps:
(1) get 100ml dodecyl triphenyl bromide phosphine solution, in the environment of-10 ℃, the 800 order natural graphite powders of 3g are dipped in solution, stir 60min, at operating frequency 45kHz, under power 160W effect, it is intermolecular that ultrasonic 1h makes solvent molecule be intercalation into graphite, obtains expansible black lead.
(2) under argon shield environment, be heated to 90 ℃ 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 3 times for filter cake, deionized water is washed till after neutrality, dries 7h and obtain black Graphene pressed powder in 60 ℃ of baking ovens.
(5) will make Graphene pressed powder and be dispersed in 100ml propyl carbinol, and at operating frequency 60kHZ, after the lower ultrasonic 50min of power 160W effect, graphene uniform will be dispersed in propyl carbinol, obtain black single-layer graphene butanol solution.
Embodiment 4
A kind of single-layer graphene organic solution preparation method, carries out according to following steps:
(1) get 100ml N-Methyl pyrrolidone solution, in the environment of-0 ℃, the 1000 order natural graphite powders of 0.5g are dipped in solution, stir 2h, at operating frequency 45kHz, under power 160W effect, it is intermolecular that ultrasonic 30min makes solvent molecule be intercalation into graphite, obtains expansible black lead.
(2) under argon shield environment, be heated to 90 ℃ and be incubated 20min, obtain expanded graphite.
(3) at operating frequency 60kHZ, under power 160W effect, expanded graphite solution is carried out to ultrasonic peeling off after 30min, 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 2h and obtain black Graphene pressed powder in 60 ℃ of baking ovens.
(5) will make Graphene pressed powder and be dispersed in 100ml dimethyl sulfoxide (DMSO), and at operating frequency 60kHZ, after the lower ultrasonic 30min of power 160W effect, graphene uniform will be dispersed in dimethyl sulfoxide (DMSO), obtain black single-layer graphene dimethyl sulphoxide solution.
Above embodiment is prepared four kinds of Graphene organic solutions wherein, because Graphene had carried out sufficient expansion process before being scattered in organic solvent, therefore can make it well be scattered in more organic solution as toluene, ethylene glycol or Virahol etc.
In the preparation process of single-layer graphene pyridine solution, the effect of selecting N-Methyl pyrrolidone or dodecyl triphenyl bromide phosphine, as intercalator, graphite is peeled off into single-layer graphene is better, individual layer rate, up to more than 99%, is easy to Graphene and is dispersed in other organic solvents.Finally, to embodiment 1, utilizing atomic power electron microscope to carry out phenogram is illustrated in figure 1 Graphene atomic force microscope picture and Figure 2 shows that Graphene altitude distribution figure; By scanning electronic microscope, characterize and be illustrated in figure 3 Graphene scanning electronic microscope schematic diagram simultaneously.Shown in Fig. 1, show that single-layer graphene layer is smooth and level and smooth, altitude distribution is shown in Fig. 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 (9)
1. a single-layer graphene organic solution preparation method, is characterized in that, according to following steps, carries out:
(1) prepare graphite solution in graphite being joined to organic solvent at-10 ~ 0 ℃, fully stir 30min ~ 2h, by the ultrasonic interlayer that makes solvent molecule be intercalation into graphite, obtain expansible black lead solution;
(2), under argon shield atmosphere, expansible black lead solution is heated to 80 ~ 100
0c, insulation 20min ~ 1h, obtains 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 pressed powder is dispersed in organic solvent through ultrasonic, obtains finely dispersed Graphene organic solution.
2. single-layer graphene organic solution preparation method according to claim 1, is characterized in that, the organic solvent described in step (1) is one or both mixtures in dodecyl triphenyl bromide phosphine or N-Methyl pyrrolidone.
3. according to the single-layer graphene organic solution preparation method described in claim l, it is characterized in that, the graphite described in step (1) is 400 ~ 1000 object natural graphite powders.
4. single-layer graphene organic solution preparation method according to claim 1, is characterized in that, the graphite concentration of polymer solution described in step (1) is 0.5% ~ 5%.
5. single-layer graphene organic 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 organic solution preparation method described in claim l, it is characterized in that, the liquid phase stripping method parameter of the ultrasonic dispersion described in step (3) is: operating frequency 60kHZ, power 160W, ultrasonic splitting time 30min ~ 2h.
7. according to the single-layer graphene organic 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, the filter cake obtaining fully washs with mass concentration 2% dilute hydrochloric acid, 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 organic solution preparation method described in claim l, it is characterized in that, the parameter of the ultrasonic dispersion described in step (5) is: at operating frequency 60kHZ, power 160W, ultrasonication time 30min ~ 2h.
9. single-layer graphene organic solution preparation method according to claim 1, is characterized in that, the organic solvent described in step (5) is the one in pyridine, dimethyl formamide, dimethyl sulfoxide (DMSO), toluene, ethylene glycol, Virahol or propyl carbinol.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104556020A (en) * | 2015-01-23 | 2015-04-29 | 青岛科技大学 | Preparation method of graphene ethanol dispersion solution |
| CN105084353A (en) * | 2015-08-19 | 2015-11-25 | 临安万杵材料科技有限公司 | Production method of graphene material |
| CN105480970A (en) * | 2016-01-11 | 2016-04-13 | 赵社涛 | Low-cost production method for sheet carbon material powder |
| CN105948033A (en) * | 2016-07-11 | 2016-09-21 | 黑龙江碳时代石墨烯科技有限公司 | Method of preparing graphene by means of wet microwave stripping |
| CN107142132A (en) * | 2017-05-26 | 2017-09-08 | 北京碳世纪科技有限公司 | Lube oil additive, lubricating oil based on grapheme material and preparation method thereof |
| CN108689402A (en) * | 2018-06-01 | 2018-10-23 | 合肥国轩高科动力能源有限公司 | A kind of method that solvent graft process prepares microdilatancy graphite |
| CN108946713A (en) * | 2018-08-17 | 2018-12-07 | 中国航发北京航空材料研究院 | A kind of graphene preparation method |
| CN108991689A (en) * | 2018-08-10 | 2018-12-14 | 江苏理工学院 | A kind of graphene aluminium sheet and its processing method, a kind of novel warm boxed cassette |
| CN110157274A (en) * | 2018-03-28 | 2019-08-23 | 山东佳星环保科技有限公司 | A kind of graphene polymer water-repellent paint masterbatch and preparation method |
| CN110776737A (en) * | 2018-07-31 | 2020-02-11 | 天津大学 | Graphene-polyimide resin heat-conducting composite material and preparation method thereof |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104556020A (en) * | 2015-01-23 | 2015-04-29 | 青岛科技大学 | Preparation method of graphene ethanol dispersion solution |
| CN105084353A (en) * | 2015-08-19 | 2015-11-25 | 临安万杵材料科技有限公司 | Production method of graphene material |
| CN105084353B (en) * | 2015-08-19 | 2018-11-13 | 杭州万杵材料科技有限公司 | A kind of production method of grapheme material |
| CN105480970A (en) * | 2016-01-11 | 2016-04-13 | 赵社涛 | Low-cost production method for sheet carbon material powder |
| CN105948033A (en) * | 2016-07-11 | 2016-09-21 | 黑龙江碳时代石墨烯科技有限公司 | Method of preparing graphene by means of wet microwave stripping |
| CN105948033B (en) * | 2016-07-11 | 2018-04-27 | 黑龙江碳时代石墨烯科技有限公司 | The method that wet method microwave stripping prepares graphene |
| CN107142132A (en) * | 2017-05-26 | 2017-09-08 | 北京碳世纪科技有限公司 | Lube oil additive, lubricating oil based on grapheme material and preparation method thereof |
| CN110157274A (en) * | 2018-03-28 | 2019-08-23 | 山东佳星环保科技有限公司 | A kind of graphene polymer water-repellent paint masterbatch and preparation method |
| CN108689402A (en) * | 2018-06-01 | 2018-10-23 | 合肥国轩高科动力能源有限公司 | A kind of method that solvent graft process prepares microdilatancy graphite |
| CN110776737A (en) * | 2018-07-31 | 2020-02-11 | 天津大学 | Graphene-polyimide resin heat-conducting composite material and preparation method thereof |
| CN108991689A (en) * | 2018-08-10 | 2018-12-14 | 江苏理工学院 | A kind of graphene aluminium sheet and its processing method, a kind of novel warm boxed cassette |
| CN108946713A (en) * | 2018-08-17 | 2018-12-07 | 中国航发北京航空材料研究院 | A kind of graphene preparation method |
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