CN113697801B - Graphene preparation method based on vortex cavitation technology - Google Patents
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Abstract
The invention discloses a graphene preparation method based on an eddy current cavitation technology, and relates to a graphene preparation method. The method aims to solve the technical problems of low yield and high equipment pressure of the existing method for preparing the graphene powder by utilizing the cavitation technology. The method comprises the following steps: firstly, building a graphene preparation device based on a vortex cavitation technology; the expanded graphite obtained by intercalating and expanding graphite powder is compressed, added into a cavitation mixing tank in a negative pressure state together with a dispersant and a solvent, then input into a vortex cavitation device for cavitation stripping, and then subjected to settling and separation to obtain the graphene dispersion liquid. The method has high graphene stripping efficiency, the graphene yield is 35-40%, and the percentage of graphene in the product with less than 10 layers is 80-85%. Can be used in the fields of materials science, micro-nano processing, energy, biomedicine and drug delivery.
Description
Technical Field
The invention relates to a preparation method of graphene.
Background
Graphene (Graphene) is sp 2 The hybridized and connected carbon atoms are tightly packed into a new material with a single-layer two-dimensional honeycomb lattice structure. Graphene has excellent optical, electrical and mechanical properties, has important applications in the aspects of materials science, micro-nano processing, energy, biomedicine, drug delivery and the like, and is considered to be a revolutionary material in the future. The method for producing graphene powder includes a mechanical stripping method, a redox method and a SiC epitaxial growth method, and the method for producing a graphene film includes a Chemical Vapor Deposition (CVD) method. Compared with other stripping methods, the mechanical stripping method for preparing graphene has the advantages of simple equipment, low cost and the like, for example, a method for preparing graphene by hydrodynamic cavitation liquid-phase stripping disclosed in a Chinese patent with the application number of CN201811024752.6 is a method for preparing graphene by utilizing a cavitation technology, and the method comprises the following steps: dispersing graphite in a solvent containing a surfactant, and fully stirring to obtain a graphite dispersion liquid; sending the graphite dispersion liquid into a cavitation element orifice plate, a venturi tube or a valve by a pump at the flow rate of 0.5-50000L/h, maintaining the cavitation pressure at 0.1-50Mpa and the system temperature at 4-50 ℃ in the cavitation process to obtain primary cavitation dispersion liquid; continuously introducing the primary cavitated dispersion liquid into a cavitation element, and repeating the cavitation operation for 1-200 times to obtain the dispersion liquid subjected to circulating cavitation; collecting the dispersion liquid after circulation cavitation, centrifuging at 500-1000rpm for 5-120min, collecting supernatant, and freeze drying to obtain the final productTo graphene powder. But the yield of the graphene powder is less than or equal to 5.6 percent, the yield is lower, and the equipment pressure is high.
Disclosure of Invention
The application aims to solve the technical problems of low yield and high equipment pressure of the existing method for preparing graphene powder by utilizing a cavitation technology, and provides a graphene preparation method based on a vortex cavitation technology.
The graphene preparation method based on the eddy current cavitation technology comprises the following steps:
1. the graphene preparation device based on the vortex cavitation technology is built: the device comprises a graphite storage tank 1, an electrochemical intercalator 2, a microwave expander 3, a compressor 4, a dispersant storage tank 5, a solvent storage tank 6, a cavitation mixing tank 7, a vortex cavitator 8, a vacuum pump 9, a filter 10 and a graphene dispersion liquid storage tank 11;
wherein the upper part of the side wall of the cavitation mixing tank 7 is provided with a feed inlet 7-1, a dispersant inlet 7-2, a solvent inlet 7-3, a cavitation liquid inlet 7-4 and a reflux port 7-5; a slurry outlet 7-6 is arranged in the middle of the side wall of the cavitation mixing tank 7; a vacuum pumping port 7-7 is arranged at the top of the cavitation mixing tank 7; a discharge port 7-8 is arranged at the bottom of the cavitation mixing tank 7;
the graphite storage tank 1 is sequentially connected with the electrochemical intercalator 2, the microwave expander 3 and the compressor 4 and then connected with a feed inlet 7-1 of the cavitation mixing tank 7;
the dispersing agent storage tank 5 is connected with a dispersing agent inlet 7-2 of the cavitation mixing tank 7;
the solvent storage tank 6 is connected with a solvent inlet 7-3 of the cavitation mixing tank 7;
the vacuum pump 9 is connected with a vacuumizing port 7-7 of the cavitation mixing tank 7;
a discharge port 7-8 of the cavitation mixing tank 7 is connected with an inlet of the vortex cavitation device 8; the outlet of the vortex cavitation device 8 is connected with a cavitation liquid inlet 7-4 of the cavitation mixing tank 7;
the filter 10 is provided with an inlet 10-1, a slag outlet 10-2 and a liquid outlet 10-3; a slurry outlet 7-6 of the cavitation mixing tank 7 is connected with an inlet 10-1 of a filter 10; a slag outlet 10-2 of the filter 10 is connected with a return port 7-5 of the cavitation mixing tank 7; a liquid outlet 10-3 of the filter 10 is connected with a graphene dispersion liquid storage tank 11;
2. graphite powder in the graphite storage tank 1 enters an electrochemical intercalator 2 for sulfuric acid intercalation to obtain expandable graphite;
3. the expandable graphite enters a microwave bulking device 3 for bulking to obtain the expanded graphite;
4. the expanded graphite enters a compressor to be compressed to obtain compressed expanded graphite;
5. injecting the compressed expanded graphite, the dispersant in the dispersant storage tank 5 and the solvent in the solvent storage tank 6 into a cavitation mixing tank 7 in proportion, maintaining the cavitation mixing tank 7 in a negative pressure state through a vacuum pump 9, and mixing to obtain a mixed solution;
6. inputting the mixed liquid in the cavitation mixing tank 7 into a vortex cavitator 8 for cavitation stripping; after cavitation stripping for 10-15 minutes, conveying the cavitation liquid to a cavitation mixing tank 7 for settlement treatment;
7. and after the sedimentation treatment is finished, opening a slurry outlet 7-6 of the cavitation mixing tank 7, conveying the slurry on the upper layer to a filter 10 for separation, conveying the separated graphene dispersion liquid to a graphene dispersion liquid storage tank, and returning the rest dispersion liquid to the cavitation mixing tank 7 for continuous cavitation stripping.
Furthermore, in the fourth step, the volume of the expanded graphite after compression is 1/20-1/50 of the original expanded graphite. The process is beneficial to the storage, transportation and next-step dispersion of the expanded graphite, and simultaneously, gaps are kept among the expanded graphite sheets, so that the solvent is ensured to enter among the expanded graphite sheets.
Furthermore, in the fifth step, the negative pressure state of the cavitation mixing tank 7 means that the vacuum degree of the cavitation mixing tank 7 is-0.04 to-0.06 MPa. Under the vacuum condition, the cavitation effect in the vortex cavitation device is facilitated.
Furthermore, in the fifth step, the dispersant is sodium cholate, sodium Dodecyl Benzene Sulfonate (SDBS) or N-methyl pyrrolidone (NMP);
further, in step five, the solvent is water, ethanol, methanol or N-methylpyrrolidone (NMP).
Further, in step five, the expanded graphite: dispersing agent: the mass ratio of the solvent is 1: (0.001-0.005): (200-500).
Furthermore, in the sixth step, the linear velocity of the middle position of the blade in the vortex cavitation device 8 is 27-40 m/s, and the outlet pressure is 0.1-0.2 MPa.
Furthermore, in the sixth step, the time of the sedimentation treatment is 4 to 8 hours.
The invention carries out sulfuric acid intercalation on graphite powder by an electrochemical intercalator, and inserts sulfuric acid between graphite sheets to obtain the expandable graphite. The intercalated expandable graphite enters a microwave bulking device, sulfuric acid is rapidly gasified through microwaves, and the sheets of graphite powder are expanded under the action of sulfuric acid volume expansion to form the expandable graphite. Then inputting the expanded graphite into an expanded graphite compressor for compression until the volume of the expanded graphite is 5% -2% of the original volume, wherein the process is favorable for next-step dispersion of the expanded graphite, and meanwhile, the sheets of the expanded graphite still have gaps; the ratio of the dispersing agent to the solvent is controlled within the range of the invention, which is beneficial to dispersion, and the dispersing agent can be attached to the surface of graphene, and cannot completely wrap the graphene, thereby affecting the performance of the graphene. The cavitation mixing tank is used for forming expanded graphite dispersion liquid, the pressure in the tank body is kept to be about-0.05 MPa through the action of a vacuum pump, and the cavitation effect is formed by the vortex cavitator under the pressure. The vortex cavitator is used for generating a cavitation effect, and the sheets of the expanded graphite are damaged and peeled off through the shearing, blasting, oscillation and other actions of the cavitation effect to form the graphene nanoplatelets. The filter is used for filtering and separating the dispersion liquid in the cavitation mixing tank to obtain the graphene dispersion liquid, the graphene dispersion liquid is input into the graphene dispersion liquid storage tank to be stored, and other dispersion liquid flows back to the cavitation mixing tank.
The graphene preparation method based on the eddy current cavitation technology is high in stripping efficiency, the graphene yield is 35% -40%, the percentage of graphene in the product with less than 10 layers is 80% -85%, and the product quality is good. The equipment has the advantages of simple operation, low pressure, low energy consumption, no environmental pollution, easy large-scale production and wide application prospect.
Drawings
Fig. 1 is a schematic diagram of a graphene preparation apparatus based on the eddy current cavitation technology according to the present invention;
FIG. 2 is a schematic structural view of a cavitation mixing tank;
FIG. 3 is a schematic view of the filter construction;
fig. 4 is a photograph and a cross-sectional graph of graphene of example 1;
fig. 5 is a photograph and a cross-sectional graph of graphene of example 4.
In the figure: 1 is a graphite storage tank, 2 is an electrochemical intercalator, 3 is a microwave expander, 4 is a compressor, 5 is a dispersant storage tank, 6 is a solvent storage tank, 7 is a cavitation mixing tank, 7-1 is a feed inlet, 7-2 is a dispersant inlet, 7-3 is a solvent inlet, 7-4 is a cavitation liquid inlet, 7-5 is a reflux port, 7-6 is a slurry outlet, 7-7 is a vacuumizing port, and 7-8 is a discharge port; 8 is a vortex cavitator, 9 is a vacuum pump, 10 is a filter, 10-1 is an inlet, 10-2 is a slag outlet, and 10-3 is a liquid outlet; and 11 is a graphene dispersion liquid storage tank.
Detailed Description
The following tests were used to demonstrate the beneficial effects of the present invention.
Example 1: the graphene preparation method based on the eddy current cavitation technology of the embodiment is carried out according to the following steps:
1. the graphene preparation device based on the vortex cavitation technology is built: the device consists of a graphite storage tank 1, an electrochemical intercalator 2, a microwave expander 3, a compressor 4, a dispersant storage tank 5, a solvent storage tank 6, a cavitation mixing tank 7, a vortex cavitator 8, a vacuum pump 9, a filter 10 and a graphene dispersion liquid storage tank 11;
wherein the upper part of the side wall of the cavitation mixing tank 7 is provided with a feed inlet 7-1, a dispersant inlet 7-2, a solvent inlet 7-3, a cavitation liquid inlet 7-4 and a reflux port 7-5; a slurry outlet 7-6 is arranged in the middle of the side wall of the cavitation mixing tank 7; a vacuumizing port 7-7 is arranged at the top of the cavitation mixing tank 7; a discharge port 7-8 is arranged at the bottom of the cavitation mixing tank 7;
the graphite storage tank 1 is sequentially connected with the electrochemical intercalator 2, the microwave expander 3 and the compressor 4 and then connected with a feeding port 7-1 of the cavitation mixing tank 7;
the dispersing agent storage tank 5 is connected with a dispersing agent inlet 7-2 of the cavitation mixing tank 7;
the solvent storage tank 6 is connected with a solvent inlet 7-3 of the cavitation mixing tank 7;
the vacuum pump 9 is connected with a vacuumizing port 7-7 of the cavitation mixing tank 7;
a discharge port 7-8 of the cavitation mixing tank 7 is connected with an inlet of the vortex cavitation device 8; the outlet of the vortex cavitation device 8 is connected with a cavitation liquid inlet 7-4 of the cavitation mixing tank 7;
the filter 10 is provided with an inlet 10-1, a slag hole 10-2 and a liquid outlet 10-3; a slurry outlet 7-6 of the cavitation mixing tank 7 is connected with an inlet 10-1 of a filter 10; a slag outlet 10-2 of the filter 10 is connected with a return port 7-5 of the cavitation mixing tank 7; a liquid outlet 10-3 of the filter 10 is connected with a graphene dispersion liquid storage tank 11;
2. the graphite powder in the graphite storage tank 1 enters an electrochemical intercalator 2 for sulfuric acid intercalation to obtain expandable graphite;
3. the expandable graphite enters a microwave bulking device 3 and is bulked for 20 seconds under the condition that the microwave frequency is 2450MHz to obtain the expandable graphite;
4. the expanded graphite enters a compressor to be compressed to obtain compressed expanded graphite; the volume of the compressed expanded graphite is 1/30 of that of the original expanded graphite;
5. the compressed expanded graphite, sodium cholate in a dispersant storage tank 5 and water in a solvent storage tank 6 are mixed according to the mass ratio of 1:0.003:300, injecting the mixture into a cavitation mixing tank 7, maintaining the vacuum degree of the cavitation mixing tank 7 at-0.05 MPa through a vacuum pump 9, and mixing to obtain a mixed solution;
6. inputting the mixed liquid in the cavitation mixing tank 7 into a vortex cavitation device 8 for cavitation stripping, wherein the linear velocity of the middle part of a blade in the cavitation device is 30m/s, the outlet pressure is controlled to be 0.15-0.18 MPa, and after 15 minutes of cavitation stripping, conveying the cavitation liquid into the cavitation mixing tank 7 for settlement treatment for 6 hours;
7. and after the sedimentation treatment is finished, opening a slurry outlet 7-6 of the cavitation mixing tank 7, conveying the slurry on the upper layer to a filter 10 for separation, conveying the separated graphene dispersion liquid to a graphene dispersion liquid storage tank, and returning the rest dispersion liquid to the cavitation mixing tank 7 for continuous cavitation stripping.
The graphene dispersion liquid product of the embodiment is detected by the national graphene product quality supervision and inspection center, and the result is that the graphene lamellar structure is complete, the section line diagram of the graphene sample shows that the height corresponding to each section line is 4.52nm, 5.69nm and 5.53nm, and the graphene sample is of a three-layer lamellar structure. The content of 10 or less layers of the graphene dispersion product of this example was 80%. The yield of graphene in this example was 35%.
Example 2: the present example is different from example 1 in that the cavitation mixing tank 7 is maintained in a normal pressure state in the fifth step, and is otherwise the same as example 1.
The graphene dispersion liquid product obtained by the embodiment has long cavitation stripping time and high energy consumption, the sheet diameter of the obtained graphene is small, and the yield is only 10%. Thereby proving that the cavitation mixing tank 7 keeps a negative pressure state, and being beneficial to improving the quality and the yield of the graphene product.
Example 3: this example is the same as example 1 except that step four was omitted, i.e., the expanded graphite was not compressed, as in example 1.
The graphene dispersion product obtained in this example has less than 40% of graphene 10 layers or less, and the yield is only 5%. Thus, the compression operation is beneficial to the dispersion of the expanded graphite, and the quality and yield of the graphene product are improved.
Example 4: the preparation method of graphene based on the eddy current cavitation technology in the embodiment comprises the following steps:
1. the built graphene preparation device based on the vortex cavitation technology is the same as that in the embodiment 1;
2. graphite powder in the graphite storage tank 1 enters an electrochemical intercalator 2 for sulfuric acid intercalation to obtain expandable graphite;
3. the expandable graphite enters a microwave bulking device 3 and is bulked for 20 seconds under the condition that the microwave frequency is 2450MHz to obtain the expandable graphite;
4. the expanded graphite enters a compressor for compression to obtain compressed expanded graphite; the volume of the compressed expanded graphite is 1/50 of that of the original expanded graphite;
5. the compressed expanded graphite, N-methyl pyrrolidone (NMP) in a dispersant storage tank 5 and water in a solvent storage tank 6 are mixed according to the mass ratio of 1:0.004: injecting the mixture into a cavitation mixing tank 7 according to the proportion of 400, maintaining the vacuum degree of the cavitation mixing tank 7 at-0.05 MPa through a vacuum pump 9, and mixing to obtain a mixed solution;
6. inputting the mixed liquid in the cavitation mixing tank 7 into a vortex cavitation device 8 for cavitation stripping, wherein the linear velocity of the middle part of a blade in the cavitation device is 35m/s, the outlet pressure is controlled to be 0.18-0.20 MPa, and after 15 minutes of cavitation stripping, conveying the cavitation liquid into the cavitation mixing tank 7 for settlement treatment for 6 hours;
7. and after the sedimentation treatment is finished, opening a slurry outlet 7-6 of a cavitation mixing tank 7, conveying the slurry on the upper layer to a filter 10 for separation, conveying the separated graphene dispersion liquid to a graphene dispersion liquid storage tank, and returning the rest dispersion liquid to the cavitation mixing tank 7 for continuous cavitation stripping.
The graphene dispersion liquid product of the embodiment is detected by the national graphene product quality supervision and inspection center, and the result is that the graphene lamellar structure is complete, the section line diagram of the graphene sample shows that the height corresponding to each section line is 1.36nm, 1.55nm and 1.50nm, and the graphene sample is of a three-layer lamellar structure. The content of 10 layers or less of the graphene dispersion liquid product of this example was 85%. The yield of graphene in this example was 38%.
Claims (8)
1. A graphene preparation method based on vortex cavitation technology is characterized by comprising the following steps:
1. the graphene preparation device based on the vortex cavitation technology is built: the device comprises a graphite storage tank (1), an electrochemical intercalator (2), a microwave expander (3), a compressor (4), a dispersant storage tank (5), a solvent storage tank (6), a cavitation mixing tank (7), a vortex cavitator (8), a vacuum pump (9), a filter (10) and a graphene dispersion liquid storage tank (11);
wherein the upper part of the side wall of the cavitation mixing tank (7) is provided with a feed inlet (7-1), a dispersant inlet (7-2), a solvent inlet (7-3), a cavitation liquid inlet (7-4) and a reflux port (7-5); a pulp outlet (7-6) is arranged in the middle of the side wall of the cavitation mixing tank (7); a vacuum pumping port (7-7) is arranged at the top of the cavitation mixing tank (7); a discharge hole (7-8) is arranged at the bottom of the cavitation mixing tank (7);
the graphite storage tank (1) is sequentially connected with the electrochemical intercalator (2), the microwave expander (3) and the compressor (4) and then is connected with a feeding hole (7-1) of the cavitation mixing tank (7);
the dispersant storage tank (5) is connected with a dispersant inlet (7-2) of the cavitation mixing tank (7);
the solvent storage tank (6) is connected with a solvent inlet (7-3) of the cavitation mixing tank (7);
the vacuum pump (9) is connected with a vacuum-pumping port (7-7) of the cavitation mixing tank (7);
a discharge port (7-8) of the cavitation mixing tank (7) is connected with an inlet of the vortex cavitation device (8); the outlet of the vortex cavitation device (8) is connected with the cavitation liquid inlet (7-4) of the cavitation mixing tank (7);
the filter (10) is provided with an inlet (10-1), a slag hole (10-2) and a liquid outlet (10-3); a slurry outlet (7-6) of the cavitation mixing tank (7) is connected with an inlet (10-1) of the filter (10); a slag outlet (10-2) of the filter (10) is connected with a return port (7-5) of the cavitation mixing tank (7); a liquid outlet (10-3) of the filter (10) is connected with a graphene dispersion liquid storage tank (11);
2. graphite powder in the graphite storage tank (1) enters an electrochemical intercalator (2) for sulfuric acid intercalation to obtain expandable graphite;
3. the expandable graphite enters a microwave bulking device (3) for bulking to obtain the expanded graphite;
4. the expanded graphite enters a compressor to be compressed to obtain compressed expanded graphite;
5. injecting the compressed expanded graphite, the dispersing agent in the dispersing agent storage tank (5) and the solvent in the solvent storage tank (6) into a cavitation mixing tank (7) in proportion, maintaining the cavitation mixing tank (7) in a negative pressure state through a vacuum pump (9), and mixing to obtain a mixed solution;
6. the mixed liquid in the cavitation mixing tank (7) is input into a vortex cavitation device (8) for cavitation stripping; after cavitation stripping for 10-15 minutes, conveying the cavitation liquid to a cavitation mixing tank (7) for settlement treatment;
7. and after the sedimentation treatment is finished, opening a slurry outlet (7-6) of the cavitation mixing tank (7), conveying the slurry on the upper layer to a filter (10) for separation, conveying the separated graphene dispersion liquid to a graphene dispersion liquid storage tank, and returning the rest dispersion liquid to the cavitation mixing tank (7) for continuous cavitation stripping.
2. The method for preparing graphene according to claim 1, wherein the volume of the expanded graphite after compression in the fourth step is 1/20 to 1/50 of the original expanded graphite.
3. The method for preparing graphene based on vortex cavitation technology according to claim 1 or 2, wherein in the fifth step, the negative pressure state of the cavitation mixing tank (7) means that the vacuum degree of the cavitation mixing tank (7) is-0.04 MPa to-0.06 MPa.
4. The method for preparing graphene according to claim 1 or 2, wherein in the fifth step, the dispersant is sodium cholate, sodium dodecyl benzene sulfonate or N-methyl pyrrolidone.
5. The method according to claim 1 or 2, wherein in the step five, the solvent is water, ethanol, methanol or N-methylpyrrolidone.
6. The method for preparing graphene based on the vortex cavitation technology according to the claim 1 or 2, wherein in the fifth step, the expanded graphite: dispersing agent: the mass ratio of the solvent is 1: (0.001-0.005): (200-500).
7. The method for preparing graphene based on vortex cavitation technology according to claim 1 or 2, wherein in the sixth step, the linear velocity of the middle position of the blade in the vortex cavitation device (8) is 27-40 m/s, and the outlet pressure is 0.1-0.2 MPa.
8. The method for preparing graphene based on vortex cavitation technology according to claim 1 or 2, wherein in the sixth step, the time of the sedimentation treatment is 4-8 hours.
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