CN108565435B - Preparation method of graphene porous particles - Google Patents
Preparation method of graphene porous particles Download PDFInfo
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- CN108565435B CN108565435B CN201810436335.6A CN201810436335A CN108565435B CN 108565435 B CN108565435 B CN 108565435B CN 201810436335 A CN201810436335 A CN 201810436335A CN 108565435 B CN108565435 B CN 108565435B
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Abstract
The invention provides a preparation method of graphene porous particles, which comprises the steps of firstly, mixing graphene oxide, graphene and water to obtain a graphene oxide/graphene dispersion liquid; then dropping the graphene oxide/graphene dispersion liquid on the surface of a hydrophobic material, dispersing the graphene oxide/graphene dispersion liquid on the surface of the hydrophobic material in a drop shape, and drying to obtain a graphene oxide/graphene composite material; and then carrying out thermal reduction on the graphene oxide/graphene composite material in a nitrogen or inert gas atmosphere to obtain the graphene porous particles. The preparation method of the graphene porous particles provided by the invention has the advantages of simple process and high yield, and is beneficial to industrial production.
Description
Technical Field
The invention relates to the technical field of graphene porous materials, in particular to a preparation method of graphene porous particles.
Background
Graphene is increasingly emphasized due to its excellent mechanical, thermal, electrical and optical properties, and has wide applications in many fields such as electronics, conductive nanocomposite materials, thin films, electromagnetic shielding and sensors. Due to the appearance of the graphene three-dimensional material, the application field of graphene is expanded, such as the application fields of catalyst carriers, energy storage, environmental protection and the like. And the graphene three-dimensional material can be conveniently integrated in the existing use system, so that the graphene three-dimensional material can be quickly applied. Among graphene three-dimensional materials, graphene porous materials are most widely applied in the fields of environmental protection, battery electrode materials, catalysis and the like.
At present, the preparation method of the graphene porous material mainly comprises a freeze drying method and a supercritical drying method. The former is to prepare graphene hydrogel firstly, freeze and freeze the graphene hydrogel after the preparation, and then directly sublimate the frozen ice into gas in a high vacuum environment so as to leave a large number of holes and obtain the graphene porous material. The latter is to prepare graphene hydrogel firstly, and then to control the pressure and temperature to make the solvent in the gel reach its own critical point in the drying process, so as to complete the supercritical conversion from liquid phase to gas phase, and obtain the graphene porous material. The two preparation processes have the disadvantages of complex and inefficient process, and therefore, the two processes are not suitable for industrial production.
Disclosure of Invention
The technical problem is as follows: the invention aims to provide a preparation method of graphene porous particles, which is simple in process and easy to operate.
The technical scheme is as follows: the invention provides a preparation method of graphene porous particles, which comprises the following steps:
(1) mixing graphene oxide, graphene and water to obtain a graphene oxide-graphene dispersion liquid;
(2) dropping the graphene oxide-graphene dispersion liquid on the surface of a hydrophobic material, dispersing the graphene oxide-graphene dispersion liquid on the surface of the hydrophobic material in a drop shape, and drying to obtain a graphene oxide-graphene composite material;
(3) and carrying out thermal reduction on the graphene oxide-graphene composite material in an inert gas atmosphere to obtain the graphene porous particles.
Preferably, the mass ratio of the graphene oxide to the graphene is 1: 0.3-7.
Preferably, the mass ratio of the graphene oxide to the graphene is 1: 3-7.
Preferably, the concentration of the graphene oxide in the graphene oxide-graphene dispersion liquid is 1-5 mg/mL.
Preferably, the hydrophobic material is a hydrophobic copper mesh, lotus leaf, polytetrafluoroethylene or heptafluoroacrylate.
Preferably, the hydrophobic material is glass, silicon wafer, metal sheet or plastic coated with low surface energy substances, and the low surface energy substances are fluorine-containing propyl cage-like silsesquioxane or dimethyl silicone oil.
Preferably, the temperature of the thermal reduction is 300-1500 ℃, and the time of the thermal reduction is 0.5-5 h.
Preferably, the temperature of the thermal reduction is 600-1200 ℃.
Preferably, the temperature of the thermal reduction is 700-900 ℃.
Has the advantages that: the invention provides a preparation method of graphene porous particles, which comprises the steps of mixing graphene oxide, graphene and water to obtain a graphene oxide-graphene dispersion liquid; then dropping the graphene oxide-graphene dispersion liquid on the surface of a hydrophobic material to enable the graphene oxide-graphene dispersion liquid to be dispersed on the surface of the hydrophobic material in a drop shape, and then drying to obtain a graphene oxide-graphene composite material; and then carrying out thermal reduction on the graphene oxide-graphene composite material in a nitrogen or inert gas atmosphere to obtain the graphene porous particles. According to the preparation method, the graphene oxide-graphene composite material is prepared by taking the graphene oxide and the graphene as raw materials, the graphene prevents the graphene oxide from being stacked in the thermal reduction process, so that the graphene porous particles are obtained, and the preparation method has the advantage of simple process; and the graphene oxide-graphene dispersion liquid is dripped on the surface of the hydrophobic material in the preparation process, and the liquid droplets cannot be adhered to the surface of the material due to the hydrophobicity of the hydrophobic material and cannot be crushed in the drying process, so that complete particles are formed, the yield is high, and the industrial production is facilitated.
Drawings
Fig. 1 is a drop-shaped graphene oxide-graphene dispersion obtained in example 1;
fig. 2 a graphene oxide-graphene composite material obtained in example 1;
fig. 3 porous particles of graphene obtained in example 1.
Fig. 4 is an internal scanning electron microscope image of the graphene porous particle obtained in example 1, which has a distinct porous structure and a large number of wrinkles.
Detailed Description
The invention provides a preparation method of graphene porous particles, which comprises the following steps:
(1) mixing graphene oxide, graphene and water to obtain a graphene oxide-graphene dispersion liquid;
(2) dropping the graphene oxide-graphene dispersion liquid on the surface of a hydrophobic material, dispersing the graphene oxide-graphene dispersion liquid on the surface of the hydrophobic material in a drop shape, and drying to obtain a graphene oxide-graphene composite material;
(3) and carrying out thermal reduction on the graphene oxide-graphene composite material in a nitrogen or inert gas atmosphere to obtain the graphene porous particles.
According to the invention, graphene oxide, graphene and water are mixed to obtain a graphene oxide-graphene dispersion solution.
In the invention, the mass ratio of the graphene oxide to the graphene is preferably 1: 0.3-7, and more preferably 1: 3-7. In the invention, because the graphene can be prevented from being stacked in the thermal reduction process, the specific surface area of the graphene porous particles can be adjusted by adjusting and controlling the mass ratio of the graphene oxide to the graphene so as to adapt to the application requirements of different fields; specifically, the specific surface area of the resulting graphene porous particles increases as the mass ratio of graphene oxide to graphene decreases.
In the invention, the concentration of the graphene oxide in the graphene oxide-graphene dispersion liquid is preferably 1-5 mg/mL, and more preferably 2-4 mg/mL. In the present invention, the above concentration is advantageous for obtaining a stable graphene oxide-graphene dispersion.
In the present invention, the graphene oxide is preferably a powdered graphene oxide or a graphene oxide dispersion liquid. The source of the graphene oxide is not particularly limited, and commercially available graphene oxide powder or graphene oxide dispersion can be directly used.
In the invention, the graphene is selected to be powdered graphene. The source of the graphene is not particularly limited, and the graphene can be obtained by directly adopting commercially available graphene powder.
The mixing order and mixing mode of the graphene oxide, the graphene and the water are not particularly limited, and the stable graphene oxide-graphene dispersion liquid can be obtained.
In the embodiment of the present invention, the mixing of the graphene oxide, the graphene and the water preferably includes the following steps:
(1) mixing graphene oxide with water, and performing ultrasonic dispersion to obtain a graphene oxide dispersion liquid;
(2) and stirring and mixing the graphene oxide dispersion liquid and graphene to obtain a graphene oxide-graphene dispersion liquid.
According to the invention, the graphene oxide is preferably mixed with water, and subjected to ultrasonic dispersion to obtain the graphene oxide dispersion liquid.
In the embodiment of the invention, the power of the ultrasonic dispersion is preferably 50W-300W, more preferably 80W-150W; the frequency of the ultrasonic dispersion is preferably 40-50 kHz; the time of ultrasonic dispersion is preferably 0.5-2 h, and more preferably 1-1.5 h.
After the graphene oxide dispersion liquid is obtained, the graphene oxide dispersion liquid and graphene are preferably stirred and mixed to obtain the graphene oxide-graphene dispersion liquid.
In the embodiment of the invention, the stirring and mixing of the graphene oxide dispersion liquid and the graphene is preferably performed by adding the graphene under the stirring state of the graphene oxide dispersion liquid, and then continuously stirring for 10-24 hours.
In the embodiment of the invention, the rotation speed of stirring is preferably 500-5000 r/min; the continuous stirring time is preferably 15-20 h.
After the graphene oxide-graphene dispersion liquid is obtained, the graphene oxide-graphene dispersion liquid is dripped on the surface of a hydrophobic material, so that the graphene oxide-graphene dispersion liquid is dispersed on the surface of the hydrophobic material in a dripping shape, and then the graphene oxide-graphene composite material is obtained after drying.
In the invention, the hydrophobic material is preferably a hydrophobic copper mesh, lotus leaf, polytetrafluoroethylene or heptafluoroacrylate; the hydrophobic material is also preferably glass, silicon wafer, metal sheet or plastic coated with low surface energy substance, and the low surface energy substance is preferably fluorine-containing propyl cage-like silsesquioxane or dimethyl silicone oil.
The size of the dropwise graphene oxide-graphene dispersion liquid dispersed on the surface of the hydrophobic material is not particularly limited, and a person skilled in the art can adjust the size of the dropwise graphene oxide-graphene dispersion liquid according to needs.
The drying mode is not particularly limited, and the graphene oxide-graphene composite material with constant weight can be obtained by adopting a conventional drying mode such as vacuum drying, forced air drying and the like. In the embodiment of the invention, the drying is air blast drying; the drying temperature is 40-80 ℃; the drying time is 4-10 h.
In the invention, in the drying process, water is slowly removed, the graphene and the graphene oxide sheet can be slowly self-assembled into solid particles under the action of capillary force, and the phenomenon of particle fracture in the subsequent thermal reduction process can be avoided.
After the drying is completed, the graphene oxide-graphene composite material is preferably taken down from the surface of the hydrophobic material, so that graphene oxide-graphene composite material particles are obtained.
After the graphene oxide-graphene composite particles are obtained, the graphene oxide-graphene composite particles are subjected to thermal reduction in a nitrogen or inert gas atmosphere to obtain graphene porous particles. In the present invention, when thermal reduction is performed in a nitrogen or inert gas atmosphere, oxygen-containing functional groups in graphene oxide are decomposed, and graphene oxide is reduced to graphene.
In the invention, the temperature of the thermal reduction is preferably 300-1500 ℃, more preferably 600-1200 ℃, and most preferably 700-900 ℃; the time of the thermal reduction is preferably 0.5-5 h, and more preferably 2-4 h.
The preparation method of the graphene porous particles provided by the present invention is described in detail with reference to the following examples, but they should not be construed as limiting the scope of the present invention.
Example 1
(1) Taking 400mL of a mixture of graphene oxide and water, and performing ultrasonic dispersion for 1h under the conditions that the power is 50Hz and the ultrasonic frequency is 42kHz to obtain a uniform and stable graphene oxide dispersion liquid; the concentration of the graphene oxide dispersion liquid is 5 mg/mL;
(2) at room temperature, adding 0.67g of graphene under the stirring state of the graphene oxide dispersion liquid, and then continuously stirring for 18h to obtain a uniform and stable graphene oxide-graphene dispersion solution; the rotating speed of the stirring is 500 rpm;
(3) dropping the graphene oxide-graphene dispersion liquid on a hydrophobic copper mesh (as shown in fig. 1); then, putting the graphene oxide into a forced air drying oven, and drying the graphene oxide at 60 ℃ for 6 hours to obtain a graphene oxide-graphene composite material (shown in figure 2);
(4) and (2) carrying out thermal reduction on the graphene oxide-graphene composite material for 2h at 300 ℃ under the protection of inert gas to obtain the graphene porous particles (as shown in figure 3).
The graphene porous particles obtained in the present embodiment are characterized by a scanning electron microscope, and the result is shown in fig. 4, and it can be clearly seen from fig. 4 that the particles are porous structures and contain a large number of wrinkles.
The specific surface area of the graphene porous particles obtained in this example was measured by BET specific surface area measurement method, and the results are shown in table 1.
Example 2
(1) Taking 400mL of a mixture of graphene oxide and water, and performing ultrasonic dispersion for 0.5h under the conditions that the power is 80W and the ultrasonic frequency is 42kHz to obtain a uniform and stable graphene oxide dispersion liquid; the concentration of the graphene oxide dispersion liquid is 5 mg/mL;
(2) at room temperature, adding 1g of graphene under the stirring state of the graphene oxide dispersion liquid, and then continuously stirring for 10 hours to obtain a uniform and stable graphene oxide/graphene dispersion solution; the rotating speed of the stirring is 3000 rpm;
(3) dropping the graphene oxide-graphene dispersion liquid on a hydrophobic stainless steel mesh (the morphology is similar to that of fig. 1); then, putting the graphene oxide into a forced air drying oven, and drying the graphene oxide at 40 ℃ for 10 hours to obtain a graphene oxide-graphene composite material (the appearance is similar to that of the graphene oxide-graphene composite material shown in the figure 2);
(4) and (3) carrying out thermal reduction on the graphene oxide-graphene composite material for 2h at 500 ℃ under the protection of inert gas to obtain graphene porous particles (the appearance is similar to that of figure 3).
The graphene porous particles obtained in the embodiment are characterized by a scanning electron microscope, the morphology is similar to that shown in fig. 4, and the pore diameter of the obtained graphene porous particles is enlarged and more wrinkles are formed.
The specific surface area of the graphene porous particles obtained in this example was measured by BET specific surface area measurement method, and the results are shown in table 1.
Example 3
(1) Taking 400mL of a mixture of graphene oxide and water, and performing ultrasonic dispersion for 2h under the conditions that the power is 150W and the ultrasonic frequency is 42kHz to obtain a uniform and stable graphene oxide dispersion liquid; the concentration of the graphene oxide dispersion liquid is 5 mg/mL;
(2) at room temperature, adding 2g of graphene under the stirring state of the graphene oxide dispersion liquid, and then continuously stirring for 24 hours to obtain a uniform and stable graphene oxide-graphene dispersion solution; the rotating speed of the stirring is 4000 rpm;
(3) dropping the graphene oxide-graphene dispersion on hydrophobic polytetrafluoroethylene (the morphology is similar to that of FIG. 1); then, putting the graphene oxide into a forced air drying oven, and drying the graphene oxide at 80 ℃ for 4 hours to obtain a graphene oxide-graphene composite material (the appearance is similar to that of the graphene oxide-graphene composite material shown in the figure 2);
(4) and (3) carrying out thermal reduction on the graphene oxide-graphene composite material for 2h at 1000 ℃ under the protection of inert gas to obtain graphene porous particles (the appearance is similar to that of figure 3).
The graphene porous particles obtained in the embodiment are characterized by a scanning electron microscope, the morphology is similar to that shown in fig. 4, and the pore diameter of the obtained graphene porous particles is enlarged and more wrinkles are formed.
The specific surface area of the graphene porous particles obtained in this example was measured by BET specific surface area measurement method, and the results are shown in table 1.
Example 4
(1) Taking 400mL of a mixture of graphene oxide and water, and performing ultrasonic dispersion for 1h under the conditions that the power is 300W and the ultrasonic frequency is 42kHz to obtain a uniform and stable graphene oxide dispersion liquid; the concentration of the graphene oxide dispersion liquid is 5 mg/mL;
(2) at room temperature, under the stirring state of the graphene oxide dispersion liquid, adding 6g of graphene, and then continuously stirring for 18h to obtain a uniform and stable graphene oxide-graphene dispersion solution; the rotating speed of the stirring is 5000 rpm;
(3) dropping the graphene oxide-graphene dispersion liquid on lotus leaves (the appearance is similar to that in figure 1), then placing the lotus leaves into a blast drying oven, and drying the lotus leaves at 60 ℃ for 6 hours to obtain a graphene oxide/graphene composite material (the appearance is similar to that in figure 2);
(4) and (3) carrying out thermal reduction on the graphene oxide-graphene composite material for 2h at 1500 ℃ under the protection of inert gas to obtain graphene porous particles (the appearance is similar to that of figure 3).
The graphene porous particles obtained in the embodiment are characterized by a scanning electron microscope, the morphology is similar to that shown in fig. 4, and the pore diameter of the obtained graphene porous particles is enlarged and more wrinkles are formed.
The specific surface area of the graphene porous particles obtained in this example was measured by BET specific surface area measurement method, and the results are shown in table 1.
Example 5
(1) Taking 400mL of a mixture of graphene oxide and water, and performing ultrasonic dispersion for 1h under the conditions that the power is 200W and the ultrasonic frequency is 42kHz to obtain a uniform and stable graphene oxide dispersion liquid; the concentration of the graphene oxide dispersion liquid is 1 mg/mL;
(2) at room temperature, adding 2g of graphene under the stirring state of the graphene oxide dispersion liquid, and then continuously stirring for 18h to obtain a uniform and stable graphene oxide-graphene dispersion solution; the rotating speed of the stirring is 5000 rpm;
(3) dropping the graphene oxide-graphene dispersion liquid on a fluorine-containing propyl cage-like silsesquioxane modified silicon wafer (the appearance is similar to that of FIG. 1); then, putting the graphene oxide/graphene composite material into a forced air drying oven, and drying the graphene oxide/graphene composite material for 6 hours at the temperature of 60 ℃ to obtain the graphene oxide/graphene composite material (the appearance is similar to that of the graphene oxide/graphene composite material shown in the figure 2);
(4) and (3) carrying out thermal reduction on the graphene oxide-graphene composite material for 2h at 900 ℃ under the protection of inert gas to obtain graphene porous particles (the appearance is similar to that of figure 3).
The graphene porous particles obtained in the embodiment are characterized by a scanning electron microscope, the morphology is similar to that shown in fig. 4, and the pore diameter of the obtained graphene porous particles is enlarged and more wrinkles are formed.
The specific surface area of the graphene porous particles obtained in this example was measured by BET specific surface area measurement method, and the results are shown in table 1.
Example 6
(1) Taking 400mL of a mixture of graphene oxide and water, and performing ultrasonic dispersion for 1h under the conditions that the power is 250W and the ultrasonic frequency is 42kHz to obtain a uniform and stable graphene oxide dispersion liquid; the concentration of the graphene oxide dispersion liquid is 3 mg/mL;
(2) at room temperature, adding 8.4g of graphene under the stirring state of the graphene oxide dispersion liquid, and then continuously stirring for 18h to obtain a uniform and stable graphene oxide-graphene dispersion solution; the rotating speed of the stirring is 2500 rpm;
(3) dropping the graphene oxide-graphene dispersion on silica-modified glass (morphology similar to figure 1); then, putting the graphene oxide into a blast drying oven, and drying the graphene oxide at 60 ℃ for 6 hours to obtain a graphene oxide-graphene composite material (the appearance is similar to that of the graphene oxide-graphene composite material shown in the figure 2);
(4) and (3) carrying out thermal reduction on the graphene oxide-graphene composite material for 2h at 700 ℃ under the protection of inert gas to obtain graphene porous particles (the appearance is similar to that of figure 3).
The graphene porous particles obtained in the embodiment are characterized by a scanning electron microscope, the morphology is similar to that shown in fig. 4, and the pore diameter of the obtained graphene porous particles is enlarged and more wrinkles are formed.
The specific surface area of the graphene porous particles obtained in this example was measured by BET specific surface area measurement method, and the results are shown in table 1.
TABLE 1 specific surface area of graphene porous particles obtained in examples 1 to 6
| Examples | Specific surface area (m)2/g) |
| 1 | 113.8 |
| 2 | 226.87 |
| 3 | 247.11 |
| 4 | 330.26 |
| 5 | 368.98 |
| 6 | 720.6 |
As is apparent from Table 1, the specific surface area of the porous graphene particles obtained in examples 1 to 6 was 113.8 to 720.6m2In examples 1 to 6, the addition amount of graphene gradually increases, and the specific surface area of the corresponding graphene porous particle also gradually increases, which indicates that the specific surface area of the graphene porous particle can be adjusted by adjusting the addition amount of graphene.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (6)
1. A preparation method of graphene porous particles is characterized by comprising the following steps:
1) mixing graphene oxide, graphene and water to obtain a graphene oxide-graphene dispersion liquid;
2) dropping the graphene oxide-graphene dispersion liquid on the surface of a hydrophobic material, dispersing the graphene oxide-graphene dispersion liquid on the surface of the hydrophobic material in a drop shape, and drying to obtain a graphene oxide-graphene composite material;
3) carrying out thermal reduction on the graphene oxide-graphene composite material in a nitrogen or inert gas atmosphere to obtain graphene porous particles;
the mass ratio of the graphene oxide to the graphene is 1: 0.3-7; the concentration of the graphene oxide in the graphene oxide-graphene dispersion liquid is 1-5 mg/mL; the temperature of the thermal reduction is 600-1500 ℃, and the time of the thermal reduction is 0.5-5 h.
2. The preparation method according to claim 1, wherein the mass ratio of the graphene oxide to the graphene is 1: 3-7.
3. The method for preparing porous graphene particles according to claim 1, wherein the hydrophobic material is a hydrophobic copper mesh, lotus leaf, polytetrafluoroethylene or heptafluoroacrylate.
4. The preparation method of the graphene porous particles according to claim 1, wherein the hydrophobic material is glass, silicon wafer, metal sheet or plastic coated with a low surface energy substance, and the low surface energy substance is fluorine-containing propyl cage-like silsesquioxane or simethicone.
5. The method for preparing porous graphene particles according to claim 1, wherein the temperature of the thermal reduction is 600 to 1200 ℃.
6. The method for preparing porous graphene particles according to claim 5, wherein the temperature of the thermal reduction is 700 to 900 ℃.
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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 |
| CN109437391B (en) * | 2018-12-29 | 2019-12-31 | 南京知化生态环境技术研究院有限公司 | Catalytic oxidation treatment method of wastewater |
| 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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