CN108565435A - A kind of preparation method of graphene porous particle - Google Patents
A kind of preparation method of graphene porous particle Download PDFInfo
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- CN108565435A CN108565435A CN201810436335.6A CN201810436335A CN108565435A CN 108565435 A CN108565435 A CN 108565435A CN 201810436335 A CN201810436335 A CN 201810436335A CN 108565435 A CN108565435 A CN 108565435A
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- H—ELECTRICITY
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- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
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- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
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Abstract
The present invention provides a kind of preparation methods of graphene porous particle, first mix graphene oxide, graphene and water, obtain graphene oxide/graphene dispersing solution；Then graphene oxide/the graphene dispersing solution is dropped in into hydrophobic material surface, graphene oxide/graphene dispersing solution is made to be scattered in hydrophobic material surface at drop-wise, then through drying, obtain graphene oxide/graphene composite material；Graphene oxide/the graphene composite material is heat-treated in nitrogen or atmosphere of inert gases again, obtains graphene porous particle.The preparation method of graphene porous particle provided by the present invention has advantage simple for process, and high yield rate, is conducive to industrialized production.
Description
Technical field
The present invention relates to the technical field of graphene porous material more particularly to a kind of preparation sides of graphene porous particle
Method.
Background technology
Graphene due to the performances such as excellent mechanics, calorifics, electrical and optical, more and more being paid attention to,
It suffers from and is widely applied in various fields such as electronics, conductive nano composite material, film, electromagnetic shielding and sensors.And stone
The appearance of black alkene three-dimensional material, expands the application field of graphene, is such as applied to catalyst carrier, energy storage and environment and protects
The fields such as shield.Also, graphene three-dimensional material can be conveniently integrated in existing use system, so as to adding quickly
With application.In graphene three-dimensional material, application of the graphene porous material in fields such as environmental protection, battery electrode material, catalysis
The most extensively.
The preparation method of graphene porous material includes mainly freeze-drying and supercritical drying at present.The former is first
Graphene hydrogel is prepared, freezing icing is carried out after complete, then under high vacuum environment, the ice directly distillation of knot is allowed to be gas, from
And a large amount of hole is left, obtain graphene porous material.The latter is first to prepare graphene hydrogel, then passes through pressure and temperature again
The control of degree makes the solvent in gel reach the critical point of itself in the drying process, and it is overcritical to gas phase to complete liquid phase
Transformation, obtains graphene porous material.Both preparation processes have the shortcomings that complex process, inefficient, therefore, both techniques
Be not suitable for very much industrialized production.
Invention content
Technical problem：The purpose of the present invention is to provide a kind of preparation method of graphene porous particle, the preparation methods
It is simple for process, it is easily operated.
Technical solution：The present invention provides a kind of preparation methods of graphene porous particle, include the following steps：
(1) graphene oxide, graphene and water are mixed, obtains graphene oxide-graphene dispersing solution；
(2) graphene oxide-graphene dispersing solution is dropped in into hydrophobic material surface, makes graphene oxide-graphene
Dispersion liquid is scattered in hydrophobic material surface at drop-wise, then through drying, obtains graphene oxide-graphene composite material；
(3) graphene oxide-graphene composite material is heat-treated in atmosphere of inert gases, obtains graphite
Alkene porous particle.
Preferably, the mass ratio of the graphene oxide and graphene is 1:0.3~7.
Preferably, the mass ratio of the graphene oxide and graphene is 1:3~7.
Preferably, in the graphene oxide-graphene dispersing solution graphene oxide a concentration of 1~5mg/mL.
Preferably, the hydrophobic material is hydrophobicity copper mesh, lotus leaf, polytetrafluoroethylene (PTFE) or seven fluorinated monomers.
Preferably, the hydrophobic material is glass, silicon chip, sheet metal or the plastics that surface is coated with low-surface energy substance,
The low-surface energy substance is the silsesquioxane of caged containing fluoropropyl or dimethicone.
Preferably, the temperature of the thermal reduction is 300~1500 DEG C, and the time of the thermal reduction is 0.5~5h.
Preferably, the temperature of the thermal reduction is 600~1200 DEG C.
Preferably, the temperature of the thermal reduction is 700~900 DEG C.
Advantageous effect：The present invention provides a kind of preparation methods of graphene porous particle, first by graphene oxide, stone
Black alkene and water mixing, obtain graphene oxide-graphene dispersing solution；Then by the graphene oxide-graphene dispersion drop
On hydrophobic material surface, graphene oxide-graphene dispersing solution is made to be scattered in hydrophobic material surface at drop-wise, then through drying,
Obtain graphene oxide-graphene composite material；Again by the graphene oxide-graphene composite material in nitrogen or indifferent gas
It is heat-treated in body atmosphere, obtains graphene porous particle.The present invention prepares oxygen using graphene oxide and graphene as raw material
Graphite alkene-graphene composite material, graphene prevents the stacking of graphene oxide during thermal reduction, and then obtains stone
Black alkene porous particle has advantage simple for process；And in preparation process by graphene oxide-graphene dispersion drop in hydrophobic
Material surface, due to the hydrophobicity of hydrophobic material, drop will not be adhered to material surface, be not in drying process it is broken,
To form complete graininess, high yield rate is conducive to industrialized production.
Description of the drawings
1 gained drop-wise graphene oxide of Fig. 1 embodiments-graphene dispersing solution；
1 gained graphene oxide of Fig. 2 embodiments-graphene composite material；
1 gained graphene porous particle of Fig. 3 embodiments.
Fig. 4 is the inner scanning electron microscope picture of 1 gained graphene porous particle of embodiment, has apparent porous knot
Structure and a large amount of fold.
Specific implementation mode
The present invention provides a kind of preparation methods of graphene porous particle, include the following steps：
(1) graphene oxide, graphene and water are mixed, obtains graphene oxide-graphene dispersing solution；
(2) graphene oxide-graphene dispersing solution is dropped in into hydrophobic material surface, makes graphene oxide-graphene
Dispersion liquid is scattered in hydrophobic material surface at drop-wise, then through drying, obtains graphene oxide-graphene composite material；
(3) graphene oxide-graphene composite material is heat-treated in nitrogen or atmosphere of inert gases, is obtained
To graphene porous particle.
The present invention mixes graphene oxide, graphene and water, obtains graphene oxide-graphene dispersing solution.
In the present invention, the mass ratio of the graphene oxide and graphene is preferably 1:0.3~7, more preferably 1:3~
7.It in the present invention, can be with since the addition of graphene can prevent stacking of graphene oxide during thermal reduction
Mass ratio by regulating and controlling graphene oxide and graphene adjusts the specific surface area of graphene porous particle, to adapt to different field
Application demand；Specifically, the specific surface area of gained graphene porous particle can be with the quality of graphene oxide and graphene
The reduction of ratio and increase.
In the present invention, the concentration of graphene oxide is preferably 1~5mg/ in the graphene oxide-graphene dispersing solution
ML, more preferably 2~4mg/mL.In the present invention, above-mentioned concentration is conducive to obtain stable graphene oxide-graphene dispersion
Liquid.
In the present invention, the graphene oxide is preferably powdered graphene oxide or graphene oxide dispersion.This
Invention is not particularly limited the source of the graphene oxide, can directly use commercially available graphene oxide powder or oxidation stone
Black alkene dispersion liquid.
In the present invention, the graphene is selected as powdery graphite alkene.The present invention is to the source of the graphene without spy
It is different to limit, directly use commercially available graphene powder.
The present invention is not particularly limited the order by merging of the graphene oxide, graphene and water and hybrid mode,
It can obtain stable graphene oxide-graphene dispersing solution.
In embodiments of the present invention, the mixing of the graphene oxide, graphene and water preferably includes following steps：
(1) graphene oxide is mixed with water, through ultrasonic disperse, obtains graphene oxide dispersion；
(2) graphene oxide dispersion is stirred with graphene, obtains graphene oxide-graphene dispersion
Liquid.
The present invention preferably mixes graphene oxide with water, through ultrasonic disperse, obtains graphene oxide dispersion.
In embodiments of the present invention, the power of the ultrasonic disperse is preferably 50W~300W, more preferably 80W~150W；
The frequency of the ultrasonic disperse is preferably 40~50kHz；The time of the ultrasonic disperse is preferably 0.5~2h, more preferably 1~
1.5h。
After obtaining graphene oxide dispersion, the present invention preferably stirs the graphene oxide dispersion and graphene mixed
It closes, obtains graphene oxide-graphene dispersing solution.
In embodiments of the present invention, the graphene oxide dispersion and graphene are stirred preferably in the oxygen
Under graphite alkene dispersion liquid stirring, graphene is added, then proceedes to stirring 10~for 24 hours.
In embodiments of the present invention, the rotating speed of the stirring is preferably 500~5000r/min；It is described continue stirring when
Between preferably 15~20h.
After obtaining graphene oxide-graphene dispersing solution, the present invention drops in the graphene oxide-graphene dispersing solution
Hydrophobic material surface makes graphene oxide-graphene dispersing solution be scattered in hydrophobic material surface at drop-wise, then through drying, obtains
To graphene oxide-graphene composite material.
In the present invention, the hydrophobic material is preferably hydrophobicity copper mesh, lotus leaf, polytetrafluoroethylene (PTFE) or seven perfluoroalkyl acrylates
Ester；The hydrophobic material is also preferably glass, silicon chip, sheet metal or the plastics that surface is coated with low-surface energy substance, described low
Surface energy substance is preferably the silsesquioxane of caged containing fluoropropyl or dimethicone.
The present invention does not have the size for being scattered in the drop-wise graphene oxide-graphene dispersing solution on the hydrophobic material surface
Particular determination, those skilled in the art can be adjusted according to the needs the size of drop-wise graphene oxide-graphene dispersing solution.
The present invention is not particularly limited the mode of the drying, using conventional drying mode as vacuum drying, air blast are dry
It is dry etc., graphene oxide-graphene composite material of constant weight can be obtained.In embodiments of the present invention, the drying is
Forced air drying；The temperature of the drying is 40~80 DEG C；The time of the drying is 4~10h.
In the present invention, in drying process, moisture slowly removes, the work of graphene and graphene oxide sector-meeting in capillary force
It is slowly self-assembled into solid graininess under, while subsequent thermal reduction process particle can be avoided fracture phenomena occur.
After completing drying, the present invention preferably takes the graphene oxide-graphene composite material from hydrophobic material surface
Under, obtain graphene oxide-graphene composite material particle.
After obtaining graphene oxide-graphene composite material particle, the present invention is compound by the graphene oxide-graphene
Material granule is heat-treated in nitrogen or atmosphere of inert gases, obtains graphene porous particle.In the present invention, in nitrogen
Or when being heat-treated in atmosphere of inert gases, the oxygen-containing functional group in graphene oxide decomposes, and graphene oxide is reduced to
Graphene.
In the present invention, the temperature of the thermal reduction is preferably 300~1500 DEG C, more preferably 600~1200 DEG C, optimal
It is selected as 700~900 DEG C；The time of the thermal reduction is preferably 0.5~5h, more preferably 2~4h.
The preparation method of graphene porous particle provided by the invention is described in detail with reference to embodiment, but
It is that they cannot be interpreted as limiting the scope of the present invention.
Embodiment 1
(1) mixture for taking 400mL graphene oxides and water is super in the condition that power is 50Hz, supersonic frequency is 42kHz
Sound disperses 1h, obtains uniform and stable graphene oxide dispersion；A concentration of 5mg/mL of the graphene oxide dispersion；
(2) at room temperature, under the stirring of graphene oxide dispersion, graphene 0.67g is added, then proceedes to stir
18h is mixed, uniform and stable graphene oxide-graphene dispersion solution is obtained；The rotating speed of the stirring is 500rpm；
(3) graphene oxide-graphene dispersing solution is dropped on hydrophobic copper mesh (as shown in Figure 1)；It is then placed in drum
In wind drying box, in 60 DEG C of dry 6h, graphene oxide-graphene composite material (as shown in Figure 2) is obtained；
(4) under inert gas protection by the graphene oxide-graphene composite material, 2h is heat-treated in 300 DEG C, obtained
To graphene porous particle object (as shown in Figure 3).
Graphene porous particle obtained by the present embodiment is characterized using scanning electron microscope, the results are shown in Figure 4, by Fig. 4
It can be clearly seen that the particulate matter is vesicular texture and contains a large amount of fold.
The specific surface area of graphene porous particle obtained by the present embodiment is tested using BET specific surface area test method, as a result
As shown in table 1.
Embodiment 2
(1) mixture for taking 400mL graphene oxides and water is super in the condition that power is 80W, supersonic frequency is 42kHz
Sound disperses 0.5h, obtains uniform and stable graphene oxide dispersion；A concentration of 5mg/mL of the graphene oxide dispersion；
(2) at room temperature, under the stirring of graphene oxide dispersion, graphene 1g is added, then proceedes to stir
10h obtains uniform and stable graphene oxide/graphene dispersion solution；The rotating speed of the stirring is 3000rpm；
(3) graphene oxide-graphene dispersing solution is dropped on hydrophobic stainless (steel) wire (pattern is similar to Fig. 1)；So
After be put into air dry oven, in 40 DEG C of dry 10h, obtaining graphene oxide-graphene composite material, (pattern is similar to figure
2)；
(4) under inert gas protection by the graphene oxide-graphene composite material, 2h is heat-treated in 500 DEG C, obtained
To graphene porous particle object (pattern is similar to Fig. 3).
Graphene porous particle obtained by the present embodiment is characterized using scanning electron microscope, as a result pattern is similar to Fig. 4, institute
The aperture for obtaining graphene porous particle becomes larger, and fold is more.
The specific surface area of graphene porous particle obtained by the present embodiment is tested using BET specific surface area test method, as a result
As shown in table 1.
Embodiment 3
(1) mixture for taking 400mL graphene oxides and water is super in the condition that power is 150W, supersonic frequency is 42kHz
Sound disperses 2h, obtains uniform and stable graphene oxide dispersion；A concentration of 5mg/mL of the graphene oxide dispersion；
(2) at room temperature, under the stirring of graphene oxide dispersion, graphene 2g is added, then proceedes to stir
For 24 hours, uniform and stable graphene oxide-graphene dispersion solution is obtained；The rotating speed of the stirring is 4000rpm；
(3) graphene oxide-graphene dispersing solution is dropped on hydrophobic polytetrafluoroethylene (PTFE) (pattern is similar to Fig. 1)；
It is then placed in air dry oven, in 80 DEG C of dry 4h, obtaining graphene oxide-graphene composite material, (pattern is similar to figure
2)；
(4) under inert gas protection by the graphene oxide-graphene composite material, 2h is heat-treated in 1000 DEG C,
Obtain graphene porous particle object (pattern is similar to Fig. 3).
Graphene porous particle obtained by the present embodiment is characterized using scanning electron microscope, as a result pattern is similar to Fig. 4, institute
The aperture for obtaining graphene porous particle becomes larger, and fold is more.
The specific surface area of graphene porous particle obtained by the present embodiment is tested using BET specific surface area test method, as a result
As shown in table 1.
Embodiment 4
(1) mixture for taking 400mL graphene oxides and water is super in the condition that power is 300W, supersonic frequency is 42kHz
Sound disperses 1h, obtains uniform and stable graphene oxide dispersion；A concentration of 5mg/mL of the graphene oxide dispersion；
(2) at room temperature, under the stirring of graphene oxide dispersion, graphene 6g is added, then proceedes to stir
18h obtains uniform and stable graphene oxide-graphene dispersion solution；The rotating speed of the stirring is 5000rpm；
(3) graphene oxide-graphene dispersing solution is dropped in on lotus leaf (pattern is similar to Fig. 1), is then placed in drum
In wind drying box, in 60 DEG C of dry 6h, obtain graphene oxide/graphene composite material (pattern is similar to Fig. 2)；
(4) under inert gas protection by the graphene oxide-graphene composite material, 2h is heat-treated in 1500 DEG C,
Obtain graphene porous particle object (pattern is similar to Fig. 3).
Graphene porous particle obtained by the present embodiment is characterized using scanning electron microscope, as a result pattern is similar to Fig. 4, institute
The aperture for obtaining graphene porous particle becomes larger, and fold is more.
The specific surface area of graphene porous particle obtained by the present embodiment is tested using BET specific surface area test method, as a result
As shown in table 1.
Embodiment 5
(1) mixture for taking 400mL graphene oxides and water is super in the condition that power is 200W, supersonic frequency is 42kHz
Sound disperses 1h, obtains uniform and stable graphene oxide dispersion；A concentration of 1mg/mL of the graphene oxide dispersion；
(2) at room temperature, under the stirring of graphene oxide dispersion, graphene 2g is added, then proceedes to stir
18h obtains uniform and stable graphene oxide-graphene dispersion solution；The rotating speed of the stirring is 5000rpm；
(3) graphene oxide-graphene dispersing solution is dropped in the silicon chip of the silsesquioxane of caged containing fluoropropyl modification
Upper (pattern is similar to Fig. 1)；It is then placed in air dry oven, in 60 DEG C of dry 6h, it is compound to obtain graphene oxide/graphene
Material (pattern is similar to Fig. 2)；
(4) under inert gas protection by the graphene oxide-graphene composite material, 2h is heat-treated in 900 DEG C, obtained
To graphene porous particle object (pattern is similar to Fig. 3).
Graphene porous particle obtained by the present embodiment is characterized using scanning electron microscope, as a result pattern is similar to Fig. 4, institute
The aperture for obtaining graphene porous particle becomes larger, and fold is more.
The specific surface area of graphene porous particle obtained by the present embodiment is tested using BET specific surface area test method, as a result
As shown in table 1.
Embodiment 6
(1) mixture for taking 400mL graphene oxides and water is super in the condition that power is 250W, supersonic frequency is 42kHz
Sound disperses 1h, obtains uniform and stable graphene oxide dispersion；A concentration of 3mg/mL of the graphene oxide dispersion；
(2) at room temperature, under the stirring of graphene oxide dispersion, graphene 8.4g is added, then proceedes to stir
18h is mixed, uniform and stable graphene oxide-graphene dispersion solution is obtained；The rotating speed of the stirring is 2500rpm；
(3) graphene oxide-graphene dispersing solution drops on silicon dioxide modified glass to (pattern is similar to figure
1)；It is then placed in air dry oven, in 60 DEG C of dry 6h, obtaining graphene oxide-graphene composite material, (pattern is similar to
Fig. 2)；
(4) under inert gas protection by the graphene oxide-graphene composite material, 2h is heat-treated in 700 DEG C, obtained
To graphene porous particle object (pattern is similar to Fig. 3).
Graphene porous particle obtained by the present embodiment is characterized using scanning electron microscope, as a result pattern is similar to Fig. 4, institute
The aperture for obtaining graphene porous particle becomes larger, and fold is more.
The specific surface area of graphene porous particle obtained by the present embodiment is tested using BET specific surface area test method, as a result
As shown in table 1.
The specific surface area of graphene porous particle obtained by 1 Examples 1 to 6 of table
| Embodiment | Specific surface area (m2/g) |
| 1 | 113.8 |
| 2 | 226.87 |
| 3 | 247.11 |
| 4 | 330.26 |
| 5 | 368.98 |
| 6 | 720.6 |
As shown in Table 1, the specific surface area of graphene porous particle obtained by Examples 1 to 6 is 113.8~720.6m2/ g, and
In Examples 1 to 6, the addition of graphene gradually increases, and the specific surface area of corresponding graphene porous particle also gradually increases
Greatly, illustrate that the adjustment by the addition of graphene can adjust the specific surface area of graphene porous particle.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications are also answered
It is considered as protection scope of the present invention.
Claims (9)
1. a kind of preparation method of graphene porous particle, which is characterized in that the preparation method includes the following steps：
1) graphene oxide, graphene and water are mixed, obtains graphene oxide-graphene dispersing solution；
2) graphene oxide-graphene dispersing solution is dropped in into hydrophobic material surface, makes graphene oxide-graphene dispersing solution
It is scattered in hydrophobic material surface at drop-wise, then through drying, obtains graphene oxide-graphene composite material；
3) graphene oxide-graphene composite material is heat-treated in nitrogen or atmosphere of inert gases, obtains stone
Black alkene porous particle.
2. the preparation method of graphene porous particle according to claim 1, which is characterized in that the graphene oxide and
The mass ratio of graphene is 1:0.3~7.
3. preparation method according to claim 2, which is characterized in that the mass ratio of the graphene oxide and graphene is
1:3~7.
4. the preparation method of graphene porous particle according to claim 1,2 or 3, which is characterized in that the oxidation stone
A concentration of 1~5mg/mL of graphene oxide in black alkene-graphene dispersing solution.
5. the preparation method of graphene porous particle according to claim 1, which is characterized in that the hydrophobic material is thin
Aqueous copper mesh, lotus leaf, polytetrafluoroethylene (PTFE) or seven fluorinated monomers.
6. the preparation method of graphene porous particle according to claim 1, which is characterized in that the hydrophobic material is table
Face is coated with glass, silicon chip, sheet metal or the plastics of low-surface energy substance, and the low-surface energy substance is caged containing fluoropropyl times
Half siloxanes or dimethicone.
7. the preparation method of graphene porous particle according to claim 1, which is characterized in that the temperature of the thermal reduction
It it is 300~1500 DEG C, the time of the thermal reduction is 0.5~5h.
8. the preparation method of graphene porous particle according to claim 7, which is characterized in that the temperature of the thermal reduction
It is 600~1200 DEG C.
9. the preparation method of graphene porous particle according to claim 8, which is characterized in that the temperature of the thermal reduction
It is 700~900 DEG C.
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Cited By (6)
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| CN109433224A (en) * | 2018-12-29 | 2019-03-08 | 知合环境（北京）有限责任公司 | A kind of Fenton's reaction catalyst and preparation method thereof |
| CN109437391A (en) * | 2018-12-29 | 2019-03-08 | 知合环境（北京）有限责任公司 | A kind for the treatment of by catalytic oxidation of waste water |
| CN109734244A (en) * | 2019-01-10 | 2019-05-10 | 知合环境（北京）有限责任公司 | A kind of sewage treatment process based on Fenton catalysis oxidation and MABR |
| CN110451491A (en) * | 2019-08-20 | 2019-11-15 | 中国航发北京航空材料研究院 | A kind of preparation method of porous graphene granular materials |
| CN111542213A (en) * | 2020-05-11 | 2020-08-14 | 向怀珍 | Manganese-zinc ferrite-graphene composite electromagnetic shielding material and preparation method thereof |
| CN112607726A (en) * | 2020-12-17 | 2021-04-06 | 泉州博银信息科技有限公司 | Graphene composite material, preparation method and application thereof |
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| CN109437391A (en) * | 2018-12-29 | 2019-03-08 | 知合环境（北京）有限责任公司 | A kind for the treatment of by catalytic oxidation of waste water |
| CN109734244A (en) * | 2019-01-10 | 2019-05-10 | 知合环境（北京）有限责任公司 | A kind of sewage treatment process based on Fenton catalysis oxidation and MABR |
| CN110451491A (en) * | 2019-08-20 | 2019-11-15 | 中国航发北京航空材料研究院 | A kind of preparation method of porous graphene granular materials |
| CN111542213A (en) * | 2020-05-11 | 2020-08-14 | 向怀珍 | Manganese-zinc ferrite-graphene composite electromagnetic shielding material and preparation method thereof |
| CN112607726A (en) * | 2020-12-17 | 2021-04-06 | 泉州博银信息科技有限公司 | Graphene composite material, preparation method and application thereof |
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