CN104085886A - Graphene and preparation method thereof - Google Patents
Graphene and preparation method thereof Download PDFInfo
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Abstract
The invention discloses graphene and a preparation method thereof. The preparation method comprises the following steps: (1) mixing graphite powder with aluminum chloride in the presence of inert gas, heating at 200-300DEG C for 5-95 hours, and then cooling down to 20-30DEG C; (2) then adding low-carbon nitro alkane, and stirring at 20-30DEG C for 3-70 hours, so as to obtain an intercalation mixture; and (3) carrying out microwave radiant heating on the intercalation mixture, so as to obtain expanded graphite, putting the expanded graphite into water and stirring intensively, so as to obtain a graphene suspension liquid. The preparation method has the advantages that (1) the operation process is simple and easy to control, the post-treatment is simple, and the quality of grapheme is high; (2) few damages are caused to environment and people; (3) the preparation method is applicable to large-scale preparation; (4) the grapheme is convenient to store and transport.
Description
Technical field
The present invention relates to technical field of nano material, particularly relate to a kind of Graphene and preparation method thereof.
Background technology
Graphene is the full carbon material of a kind of widely used two dimension, but prepare in a large number this material, still has the problem that cost is high.Most reports are Graphenes that preparation after graphite oxidation is contained to a large amount of defects and functional group, minority reports that useful electrochemical process or graphite graft process obtain Graphene, wherein with graft process, preparing the intercalated material that Graphene uses is metallic lithium, butyllithium or iron(ic) chloride, the above two materials are not only expensive, and it is inflammable easily sudden and violent to meet water, then a kind of material needs higher temperature when intercalation, and iron(ic) chloride is to plant and instrument seriously corroded, again with graphite in carbon atom interact very strong, therefore, not only preparation process is very complicated, and aftertreatment is also very loaded down with trivial details and difficult, be difficult to graphite simply to peel off and obtain high-quality Graphene.
Summary of the invention
In view of this, the object of the invention is to propose a kind of preparation method of Graphene, obviously to simplify the preparation process of Graphene, improve the quality of Graphene simultaneously.
Based on above-mentioned purpose, the preparation method of Graphene provided by the invention comprises the following steps:
1) graphite composite powder is mixed with aluminum chloride, under protection of inert gas, under 200～300 ℃ of conditions, heat 5～95 hours, be then cooled to 20～30 ℃;
2) continue to add low-carbon (LC) nitroparaffins, under 20～30 ℃ of conditions, stir 3～70 hours, obtain intercalation mixture;
3) intercalation mixture described in employing carry out microwave radiation heating, obtains expanded graphite powder, then this expanded graphite is placed in to water strong stirring, makes graphene suspension.
Alternatively, the mass ratio of described graphite composite powder and aluminum chloride is 1:3～10.
Preferably, described graphite composite powder is 2～10 grams per milliliters with the ratio of the quality volume of low-carbon (LC) nitroparaffins.
Preferably, described low-carbon (LC) nitroparaffins are selected from least one in Nitromethane 99Min., nitroethane and nitropropane.
Alternatively, described step 2) stirring velocity in is 500～2000 revs/min, described step 3) in stirring velocity be 6000～15000 revs/min.
Preferably, described step 4) also comprise afterwards: after described graphene suspension is centrifugal, vacuum-drying, obtain graphene powder.
Alternatively, heated mixt to 200～350 ℃ under microwave radiation, and keep 2～10 minutes.
Preferably, described microwave radiation is carried out in air, and the wavelength of described microwave is 100～200mm, and frequency is 2200～2800MHz.
The present invention also provides a kind of Graphene, and described Graphene makes according to the preparation method of above-mentioned Graphene.
As can be seen from above, graphene preparation method provided by the invention, by graphite is mixed with Aluminum chloride anhydrous, heats in rare gas element, and aluminum chloride molecule just can be inserted into graphite layers and make aluminum chloride intercalation thing under lower temperature of reaction; By aluminum chloride molecule between small organic molecule part substituted layer, under heating, make organic substance decomposing, and then allow graphite expansion peel off, thereby make Graphene again.Or directly microwave heating aluminum chloride intercalation thing, because aluminum chloride gasifies and makes expanded graphite rapidly, thereby makes Graphene.Unstable owing to being in the aluminum chloride molecule of interlayer, a little less than carbon atom in aluminum chloride and graphite interacts, there is part exchange in easy and low-carbon (LC) nitroparaffins, and then make low-carbon (LC) nitroparaffins be embedded in graphite layers, under heating condition, make the low-carbon (LC) nitroparaffins of interlayer decompose, impel graphite expansion and peel off afterwards just can make high-quality Graphene.Therefore, preparation method's tool provided by the invention has the following advantages: (1) operating process simply, easily control, aftertreatment is simple, the quality of Graphene is high; (2) little to environment and people's hazardness; (3) proper scaleization preparation; (4) be convenient to storage and transportation.
Accompanying drawing explanation:
Fig. 1 is the scanning electron microscope diagram of raw materials used graphite composite powder under 100 multiples in the embodiment of the present invention;
Fig. 2 is the scanning electron microscope diagram of raw materials used graphite composite powder under 500 multiples in the embodiment of the present invention;
Fig. 3 is the scanning electron microscope diagram of raw materials used graphite composite powder under 1000 multiples in the embodiment of the present invention
Fig. 4 is the scanning electron microscope diagram of the Graphene that makes of the embodiment of the present invention under 500 multiples;
Fig. 5 is the scanning electron microscope diagram of the Graphene that makes of the embodiment of the present invention under 1000 multiples;
Fig. 6 is the scanning electron microscope diagram of the Graphene that makes of the embodiment of the present invention under 100000 multiples;
Fig. 7 is the transmission electron microscope figure of the Graphene that makes of the embodiment of the present invention;
Fig. 8 is the X ray diffracting spectrum of embodiment of the present invention raw material sheet graphite composite powder and the Graphene making.
Embodiment
For making the object, technical solutions and advantages of the present invention clearer, below in conjunction with specific embodiment, and with reference to accompanying drawing, the present invention is described in more detail.
Embodiment 1
First, under high pure nitrogen protection, by 2 grams of graphite composite powders and 16 grams of anhydrous AlCl
3join in reactor and mix, at 250 ℃, heat 63 hours; Naturally cool to after 25 ℃, continue to add 10 milliliters of Nitromethane 99Min.s in reactor, the speed stirring with 1500 revs/min at 25 ℃ was taken out intercalation mixture after 29 hours from reactor; Then in air, under microwave radiation, heat intercalation mixture to 260 ℃ left and right, and keep 4 minutes, obtain expanded graphite; Finally, the expanded graphite after microwave heating is placed in to water and with the speed of 8500 revs/min, stirs, make the graphene suspension of favorable dispersity, after Graphene suspension liquid is centrifugal, vacuum-drying, obtain graphene powder.Preferably, described aluminum chloride is Aluminum chloride anhydrous.Wherein, the wavelength of described microwave is 150mm, and frequency is 2200MHz.It should be noted that, also can directly intercalation mixture be put into microwave oven, in air, under normal pressure, microwave heating obtains expanded graphite.
Embodiment 2
First, under high-purity argon gas protection, by 2 grams of graphite composite powders and 17 grams of anhydrous AlCl
3join in reactor and mix, at 290 ℃, heat 26 hours; Naturally cool to after 27 ℃, continue to add 15 milliliters of Nitromethane 99Min.s in reactor, the speed stirring with 650 revs/min at 26 ℃ was taken out intercalation mixture after 29 hours from reactor; Then in air, under microwave radiation, heat intercalation mixture to 220 ℃ left and right, and keep 5 minutes, obtain expanded graphite; Finally, the expanded graphite after microwave heating is placed in to water and with the speed of 10000 revs/min, stirs, make the graphene suspension of favorable dispersity, after Graphene suspension liquid is centrifugal, vacuum-drying, obtain graphene powder.Wherein, the wavelength of described microwave is 125mm, and frequency is 2600MHz.
Embodiment 3
First, under high pure nitrogen protection, by 3 grams of graphite composite powders and 25 grams of anhydrous AlCl
3join in reactor and mix, at 260 ℃, heat 52 hours; Naturally cool to after 23 ℃, continue to add 16 milliliters of Nitromethane 99Min.s in reactor, the speed stirring with 550 revs/min at 27 ℃ was taken out intercalation mixture after 62 hours from reactor; Then in air, under microwave radiation, heat intercalation mixture to 250 ℃ left and right, and keep 4.5 minutes, obtain expanded graphite; Finally, the expanded graphite after microwave heating is placed in to water and with the speed of 10650 revs/min, stirs, make the graphene suspension of favorable dispersity, after Graphene suspension liquid is centrifugal, vacuum-drying, obtain graphene powder.Wherein, the wavelength of described microwave is 130mm, and frequency is 2400MHz.It should be noted that, also can directly intercalation mixture be put into microwave oven, in air, under normal pressure, microwave heating obtains expanded graphite.
Embodiment 4
First, under high pure nitrogen protection, by 5 grams of graphite composite powders and 25 grams of anhydrous AlCl
3join in reactor and mix, at 300 ℃, heat 17 hours; Naturally cool to after 28 ℃, continue to add 16 milliliters of nitroethanes in reactor, the speed stirring with 820 revs/min at 27 ℃ was taken out intercalation mixture after 55 hours from reactor; Then in air, under microwave radiation, heat intercalation mixture to 300 ℃ left and right, and keep 4 minutes, obtain expanded graphite; Finally, the expanded graphite after microwave heating is placed in to water and with the speed of 12360 revs/min, stirs, make the graphene suspension of favorable dispersity, after Graphene suspension liquid is centrifugal, vacuum-drying, obtain graphene powder.
Embodiment 5
First, under high pure nitrogen protection, by 2.5 grams of graphite composite powders and 18 grams of anhydrous AlCl
3join in reactor and mix, at 265 ℃, heat 24 hours; After naturally cooling to 25.2 ℃, take out, heated mixt to 230 ℃ left and right under microwave radiation in air, and keep 4 minutes, obtain expanded graphite; Finally, the expanded graphite after microwave heating is placed in to water with 11000 revs/min of stirrings, makes the graphene suspension of favorable dispersity, after Graphene suspension liquid is centrifugal, vacuum-drying, obtain graphene powder.Wherein, the wavelength of described microwave is 110～160mm, and frequency is 2300～2600MHz.
Embodiment 6
First, under high pure nitrogen protection, by 2.5 grams of graphite composite powders and 25 grams of anhydrous AlCl
3join in reactor and mix, at 290 ℃, heat 25 hours; Naturally cool to after 25.2 ℃, continue to add 16 milliliters of nitroethanes in reactor, the speed stirring with 1580 revs/min at 27 ℃ was taken out intercalation mixture after 72 hours from reactor; Then in air, under microwave radiation, heat intercalation mixture to 250 ℃ left and right, and keep 4 minutes, obtain expanded graphite; Finally, the expanded graphite after microwave heating is placed in to water and with the speed of 9250 revs/min, stirs, make the graphene suspension of favorable dispersity, after Graphene suspension liquid is centrifugal, vacuum-drying, obtain graphene powder.Wherein, the wavelength of described microwave is 122mm, and frequency is 2250MHz.It should be noted that, also can directly intercalation mixture be put into microwave oven, in air, under normal pressure, microwave heating obtains expanded graphite.
Embodiment 7
First, under high pure nitrogen protection, by 3 grams of graphite composite powders and 28 grams of anhydrous AlCl
3join in reactor and mix, at 283 ℃, heat 36 hours; Naturally cool to after 26.2 ℃, continue to add 13 milliliters of nitropropanes in reactor, at 27 ℃, with 1260 revs/min of stirrings, after 70 hours, from reactor, take out intercalation mixture; Then in air, under microwave radiation, heat intercalation mixture to 260 ℃ left and right, and keep 4.8 minutes, obtain expanded graphite; Finally, the expanded graphite after microwave heating is placed in to water and with the speed of 14400 revs/min, stirs, make the graphene suspension of favorable dispersity, after Graphene suspension liquid is centrifugal, vacuum-drying, obtain graphene powder.Wherein, the wavelength of described microwave is 160mm, and frequency is 2650MHz.It should be noted that, also can directly intercalation mixture be put into microwave oven, in air, under normal pressure, microwave heating obtains expanded graphite.
Embodiment 8
First, under high-purity argon gas protection, by 4 grams of graphite composite powders and 25 grams of anhydrous AlCl
3join in reactor and mix, at 200 ℃, heat 95 hours; Naturally cool to after 25 ℃, continue to add 30 milliliters of nitropropanes in reactor, the speed stirring with 520 revs/min at 26 ℃ was taken out intercalation mixture after 50 hours from reactor; Then in air, under microwave radiation, heat intercalation mixture to 255 ℃ left and right, and keep 4.8 minutes, obtain expanded graphite; Finally, the expanded graphite after microwave heating is placed in to water and with the speed of 7700 revs/min, stirs, make the graphene suspension of favorable dispersity, after Graphene suspension liquid is centrifugal, vacuum-drying, obtain graphene powder.Wherein, the wavelength of described microwave is 135mm, and frequency is 2440MHz.
Embodiment 9
First, under high pure nitrogen protection, by 3 grams of graphite composite powders and 25 grams of anhydrous AlCl
3join in reactor and mix, at 250 ℃, heat 63 hours; After naturally cooling to 25 ℃, take out, heated mixt to 260 ℃ left and right under microwave radiation in air, and keep 5 minutes, obtain expanded graphite; Finally, the expanded graphite after microwave heating is placed in to water and with the speed of 12000 revs/min, stirs, make dispersed graphene suspension preferably, after Graphene suspension liquid is centrifugal, vacuum-drying, obtain graphene powder.Wherein, the wavelength of described microwave is 120～150mm, and frequency is 2400～2560MHz.
Referring to Fig. 1～3, be respectively the scanning electron microscope diagram of raw materials used graphite composite powder under 100 multiples, 500 multiples and 1000 multiples in the embodiment of the present invention; Referring to Fig. 4～7, be respectively scanning electron microscope diagram and the transmission electron microscope figure of the Graphene that makes of the embodiment of the present invention under 500 multiples, 1000 multiples and 100000 multiples.
As can be seen from the figure, raw material graphite is to have sheet-like morphology, and size is the phosphorus flake graphite between 0.2～0.4mm mainly, and thickness is also very thick.The Graphene preparing by method provided by the invention thickness is very thin, has obvious fold to exist.
Referring to Fig. 8, it is the X ray diffracting spectrum of embodiment of the present invention raw material graphite composite powder with the Graphene making; As can be seen from the figure, the X-ray diffraction peak intensity of raw material graphite composite powder is strong especially, is far better than the intensity at the X-ray diffraction peak of prepared Graphene, and this is due to Graphene, to have the cause of individual layer or which floor structure of minority.
As mentioned above, graphene preparation method provided by the invention, by graphite is mixed with Aluminum chloride anhydrous, heats in rare gas element, and aluminum chloride molecule just can be inserted into graphite layers and make aluminum chloride intercalation thing under lower temperature of reaction; By aluminum chloride molecule between small organic molecule part substituted layer, under heating, make organic substance decomposing, and then allow graphite expansion peel off, thereby make Graphene again.Or directly microwave heating aluminum chloride intercalation thing, because aluminum chloride gasifies and makes expanded graphite rapidly, thereby makes Graphene.Unstable owing to being in the aluminum chloride molecule of interlayer, a little less than carbon atom in aluminum chloride and graphite interacts, there is part exchange in easy and low-carbon (LC) nitroparaffins, and then make low-carbon (LC) nitroparaffins be embedded in graphite layers, under heating condition, make the low-carbon (LC) nitroparaffins of interlayer decompose, impel graphite expansion and peel off afterwards just can make high-quality Graphene.Therefore, preparation method's tool provided by the invention has the following advantages: (1) operating process simply, easily control, aftertreatment is simple, the quality of Graphene is high; (2) little to environment and people's hazardness; (3) proper scaleization preparation; (4) be convenient to storage and transportation.
Those of ordinary skill in the field are to be understood that: the foregoing is only specific embodiments of the invention; be not limited to the present invention; within the spirit and principles in the present invention all, any modification of making, be equal to replacement, improvement etc., within all should being included in protection scope of the present invention.
Claims (9)
1. a preparation method for Graphene, is characterized in that, comprises the following steps:
1) graphite composite powder is mixed with aluminum chloride, under protection of inert gas, under 200～300 ℃ of conditions, heat 5～95 hours, be then cooled to 20～30 ℃;
2) continue to add low-carbon (LC) nitroparaffins, under 20～30 ℃ of conditions, stir 3～70 hours, obtain intercalation mixture;
3) intercalation mixture described in employing carry out microwave radiation heating, obtains expanded graphite, then this expanded graphite is placed in to water strong stirring, makes graphene suspension.
2. the preparation method of Graphene according to claim 1, is characterized in that, the mass ratio of described graphite composite powder and aluminum chloride is 1:3～10.
3. the preparation method of Graphene according to claim 1, is characterized in that, described graphite composite powder is 2～10 grams per milliliters with the ratio of the quality volume of low-carbon (LC) nitroparaffins.
4. the preparation method of Graphene according to claim 3, is characterized in that, described low-carbon (LC) nitroparaffins are selected from least one in Nitromethane 99Min., nitroethane and nitropropane.
5. the preparation method of Graphene according to claim 1, is characterized in that, described step 2) in stirring velocity be 500～2000 revs/min, described step 3) in stirring velocity be 6000～15000 revs/min.
6. the preparation method of Graphene according to claim 1, is characterized in that, described step 4) also comprise afterwards: after described graphene suspension is centrifugal, vacuum-drying, obtain graphene powder.
7. the preparation method of Graphene according to claim 1, is characterized in that, heated mixt to 200～350 ℃ under microwave radiation, and keep 2～10 minutes.
8. the preparation method of Graphene according to claim 1, is characterized in that, described microwave radiation is carried out in air, and the wavelength of described microwave is 100～200mm, and frequency is 2200～2800MHz.
9. a Graphene, is characterized in that, described Graphene makes according to the preparation method of the Graphene described in any one in claim 1～8.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104477886A (en) * | 2014-11-20 | 2015-04-01 | 中山大学 | Folded graphene and controllable preparation method thereof |
| CN104556010A (en) * | 2014-12-31 | 2015-04-29 | 江苏江大环保科技开发有限公司 | Process for industrially producing graphene by microwaves |
| CN104817074A (en) * | 2015-04-20 | 2015-08-05 | 德阳烯碳科技有限公司 | Process for preparing graphite intercalation compound |
| CN105293482A (en) * | 2015-12-01 | 2016-02-03 | 张扬威 | Solvothermal stripping preparation method of graphene |
| CN106672958A (en) * | 2017-01-18 | 2017-05-17 | 丽水市知科科技有限公司 | Preparation method of graphene oxide |
| CN106744888A (en) * | 2017-01-18 | 2017-05-31 | 丽水市知科科技有限公司 | A kind of preparation method of Graphene |
| CN108622886A (en) * | 2017-03-17 | 2018-10-09 | 国家纳米科学中心 | A kind of liquid nitrogen auxiliary prepares the method for high-quality graphene and high-quality graphene obtained |
| CN113493200A (en) * | 2020-10-17 | 2021-10-12 | 苏州北美国际高级中学 | Preparation method of graphene oxide |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104477886A (en) * | 2014-11-20 | 2015-04-01 | 中山大学 | Folded graphene and controllable preparation method thereof |
| CN104477886B (en) * | 2014-11-20 | 2016-09-28 | 中山大学 | A kind of accordion Graphene and controllable method for preparing thereof |
| CN104556010A (en) * | 2014-12-31 | 2015-04-29 | 江苏江大环保科技开发有限公司 | Process for industrially producing graphene by microwaves |
| CN104817074A (en) * | 2015-04-20 | 2015-08-05 | 德阳烯碳科技有限公司 | Process for preparing graphite intercalation compound |
| CN105293482A (en) * | 2015-12-01 | 2016-02-03 | 张扬威 | Solvothermal stripping preparation method of graphene |
| CN106672958A (en) * | 2017-01-18 | 2017-05-17 | 丽水市知科科技有限公司 | Preparation method of graphene oxide |
| CN106744888A (en) * | 2017-01-18 | 2017-05-31 | 丽水市知科科技有限公司 | A kind of preparation method of Graphene |
| CN108622886A (en) * | 2017-03-17 | 2018-10-09 | 国家纳米科学中心 | A kind of liquid nitrogen auxiliary prepares the method for high-quality graphene and high-quality graphene obtained |
| CN113493200A (en) * | 2020-10-17 | 2021-10-12 | 苏州北美国际高级中学 | Preparation method of graphene oxide |
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