CN111717912A - Device and method for preparing graphene through continuous stripping - Google Patents
Device and method for preparing graphene through continuous stripping Download PDFInfo
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- CN111717912A CN111717912A CN202010548166.2A CN202010548166A CN111717912A CN 111717912 A CN111717912 A CN 111717912A CN 202010548166 A CN202010548166 A CN 202010548166A CN 111717912 A CN111717912 A CN 111717912A
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Abstract
The invention discloses a device and a method for preparing graphene through continuous stripping. The device comprises a stripping module, a lifting module, a driving module and a control module of the vertical double-roller column; the peeling module is provided with a heater, a first roller and a second roller; the first roller and the second roller are arranged side by side in a gap of 0.3-0.4 cm, and the gap between the outer walls of the first roller and the second roller and the inner wall of the roller is 0.3-0.4 cm; the outer wall of the first roller is provided with threads with the thread pitch of 0.2-0.3 cm and the depth of 0.2-0.3 cm, and the outer wall of the second roller is smooth. The method utilizes the adhesive to treat the graphite powder, and is green, safe and low in cost; the device is combined again, the defect that the feeding and discharging of the traditional preparation process need to be stopped is overcome, the uninterrupted continuous work of feeding, stripping, discharging, re-feeding, stripping and re-discharging is realized, and the industrial practicability is good.
Description
Technical Field
The invention belongs to the technical field of graphene, and particularly relates to a device and a method for preparing graphene through continuous stripping.
Background
Since 2004, single-layer graphene is prepared by using a micro-mechanical stripping method for the first time in laboratories of the university of manchester in the united kingdom, graphene serves as the thinnest and the hardest nano material at present, and has the advantages of high heat conductivity coefficient, high electron mobility, large specific surface area, good light transmittance, high mechanical strength and the like, so that the graphene becomes a new material in various fields such as heat dissipation of electronic components, sensors, supercapacitors, lithium batteries, material enhancement, biomedicine and the like, and is favored by scientific research workers.
To date, there are many methods and approaches for producing graphene, but the most common method is to use redox to prepare graphene. Although the method is simple and low in cost, and is suitable for mass preparation, the graphene prepared by the method usually has more structural defects, and the performance is seriously influenced. Meanwhile, more toxic reagents are involved in the preparation process, and the preparation method has great potential harm to human bodies and natural environment.
For another example, although the chemical vapor deposition method can prepare high-quality graphene, the cost is high and the energy consumption is large; the epitaxial growth method is difficult to prepare large-area graphene, the film is not uniform, and the preparation cost is high; the liquid phase stripping method is difficult to obtain single-layer graphene, and the graphite structure may be damaged in the intercalation process; the organic synthesis method starts from aromatic micromolecules, and synthesizes the polycyclic aromatic hydrocarbon or the graphene nanoribbon by one step through organic synthesis reaction, but the method has poor controllability and is not suitable for large-scale production.
And the mechanical method can realize large-scale low-cost preparation of graphene, such as the stripping of graphite by mechanical impact of ball milling, jet milling and the like. Although graphene can be obtained by mechanical grinding, the grinding impact process can damage graphite crystal lattices to a certain extent, so that the graphene layer has structural defects. Meanwhile, the existing mechanical stripping equipment is usually in an intermittent type mode, cannot work continuously, is low in yield and high in cost, and limits the application of a mechanical method in industry.
Disclosure of Invention
The invention aims to overcome the defects of the prior art, provides a device and a method for preparing graphene by continuous stripping, and solves the problems in the background art.
The technical scheme adopted by the invention for solving the technical problems is as follows: the device for preparing graphene by continuous stripping comprises a stripping module, a lifting module, a driving module and a control module;
the peeling module comprises a roller, the roller is provided with a heater, and a first roller column and a second roller column are arranged in the roller; the first roller and the second roller are arranged side by side in a gap of 0.3-0.4 cm, and the gap between the outer walls of the first roller and the second roller and the inner wall of the roller is 0.3-0.4 cm; the outer wall of the first roller is provided with threads with the thread pitch of 0.2-0.3 cm and the depth of 0.2-0.3 cm, and the outer wall of the second roller is smooth;
the driving module is connected with the first roller and the second roller;
the lifting module is used for controlling the heights of the first roller and the second roller;
the control module is connected with the stripping module, the lifting module and the driving module and used for supplying power and controlling the temperature of the roller and the rotating speed and the height of the first roller and the second roller.
In a preferred embodiment of the invention, the roller is provided with a feeding hole, an upper discharging hole and a lower discharging hole, the feeding hole and the upper discharging hole are positioned at the upper part of the roller at one side of the first roller, and the lower discharging hole is positioned at the lower part of the roller at one side of the second roller.
In a preferred embodiment of the present invention, the cross section of the upper discharge hole is square, and the cross section of the lower discharge hole is circular.
In a preferred embodiment of the invention, the clearance between the outer walls of the first roller and the second roller and the inner wall of the roller is 0.4cm, the outer wall of the first roller is provided with a thread with the thread pitch of 0.2cm and the depth of 0.2cm, and the clearance between the first roller and the second roller is 0.3 cm.
In a preferred embodiment of the present invention, the control module includes a control panel, and the control panel is provided with a power switch, a temperature adjustment window, and a rotation speed adjustment window.
The invention also provides a method for preparing graphene by continuous stripping, which adopts the device and comprises the following specific steps:
(1) mixing graphite powder and an adhesive in a ratio of 0.1-1: mixing the components in a mass ratio of 10-200 to obtain an adhesive containing graphite powder; the adhesive comprises one of polyvinyl alcohol, honey, isopropanol, sucrose, maltose and polyvinyl alcohol; the graphite powder is one of crystalline flake graphite, expanded graphite, thermal cracking graphite or graphite oxide;
(2) adding an adhesive containing graphite powder into a roller from a feed inlet of a device for stripping, wherein the stripping temperature is 25-200 ℃, and the stripping rotating speed is 100-200 rpm;
(3) the materials on the outer wall of the first roller are collected through the upper discharging hole, the stripping device is washed by deionized water, the residual materials are collected through the lower discharging hole, and the materials collected twice are mixed and then purified to obtain a graphene product.
In a preferred embodiment of the present invention, the graphite powder in the step (1) has a size of 50 to 8000 meshes.
In a preferred embodiment of the present invention, when the adhesive is polyvinyl alcohol, honey and isopropyl alcohol, the peeling temperature is 20 to 25 ℃.
In a preferred embodiment of the present invention, when the adhesive is sucrose or maltose, the peeling temperature is 150 to 200 ℃.
In a preferred embodiment of the present invention, the purification process in step (3) comprises the following steps: and standing the mixed material, carrying out ultrasonic treatment on the upper-layer dispersion liquid with the power of 1000-1100W and the frequency of 20-25 kHz for 5-10 min, and then filtering, centrifuging and drying.
Compared with the background technology, the technical scheme has the following advantages:
1. according to the invention, the graphite powder is stripped through the shearing force between the roller column and the inner wall of the roller and the shearing force between the roller columns under the action of the adhesive by adopting a vertical double-roller stripping device, and the circulation is repeated, so that the graphite powder is completely stripped, the degree of damage to the graphite crystal structure by methods such as ball milling and the like is reduced, and finally, high-quality few-layer graphene can be obtained;
2. according to the process method for realizing continuous stripping, raw materials are added from the feeding hole, after stripping for a period of time, products flow out from the discharging hole, and continuous graphite stripping is realized, namely the whole process of feeding-stripping-discharging-re-feeding-stripping-re-discharging is continuous, so that the defect that the feeding and discharging of equipment such as a traditional ball mill and the like need to be stopped is overcome, the process flow is greatly shortened, and the problem that the mass production of graphene is difficult at the present stage is effectively solved.
3. The method is simple and efficient to operate, the selected adhesive is low in cost, the use of toxic reagents is avoided, the environmental pressure is relieved to a certain extent, the problems that waste liquid is difficult to treat in the graphene preparation process at the present stage and the like can be effectively solved, and the method has good industrial practicability.
Drawings
FIG. 1 is a side view of the apparatus of example 1;
FIG. 2 is a front view of the apparatus of example 1;
fig. 3 is an SEM image of the raw material (a) used in example 2 and the prepared graphene (b).
Figure 4 is an XRD pattern of the sample obtained with the starting material used in example 2 and different stripping times.
FIG. 5 is a Raman plot of the raw material used in example 2 and samples taken at different stripping times.
Fig. 6 is an AFM image of graphene prepared in example 2.
The device comprises a control module 1, a lifting module 2, a driving module 3, a stripping module 4, a power switch 5, a rotating speed adjusting window 6, a temperature adjusting window 7, a feed inlet 8, an upper discharge outlet 9, a lower discharge outlet 10, a second roller 11, a first roller 12, a screw thread 13 and a roller 14.
Detailed Description
Example 1
Referring to fig. 1 and 2, the device for preparing graphene by continuous stripping in this embodiment includes a stripping module 4, a lifting module 2, a driving module 3, and a control module 1;
the peeling module 4 comprises a roller 14, the roller 14 is provided with a heater, and a first roller 12 and a second roller 11 are arranged in the roller 14; the first roller 12 and the second roller 11 are arranged side by side with a gap of 0.3cm, and the gap between the outer walls of the first roller 12 and the second roller 11 and the inner wall of the roller 14 is 0.4 cm; the outer wall of the first roller 12 is provided with a thread 13 with the thread pitch of 0.2cm and the depth of 0.2cm, and the outer wall of the second roller 11 is smooth;
the driving module 3 is connected to the tops of the first roller 12 and the second roller 11;
the lifting module 2 is connected with the driving module 3 and is used for controlling the heights of the first roller 12 and the second roller 11;
the control module 1 is connected with the stripping module 4, the lifting module 2 and the driving module 3; the control module 1 comprises a control panel, wherein a power switch 5, a temperature adjusting window 7 and a rotating speed adjusting window 6 are arranged on the control panel and used for supplying power and controlling the temperature of the roller 14 and the rotating speed of the first roller 12 and the second roller 11.
In this embodiment, the roller 14 is provided with a feeding hole 8, an upper discharging hole 9 and a lower discharging hole 10, the feeding hole 8 and the upper discharging hole 9 are located at the upper part of the roller 14 at one side of the first roller 12, and the lower discharging hole 10 is located at the lower part of the roller 14 at one side of the second roller 11. The section of the upper discharging port 9 is square, and when the stripping time is finished, the scraper is fixed conveniently, and the distance between the scraper and the surface of the roller is controlled to scrape the materials. The cross-section of the lower discharge opening 10 is circular to facilitate cleaning and collection of residual material on the surface of the roll.
Example 2
A method for preparing graphene by continuous stripping is to prepare the device in example 1, and prepare graphene by the following steps:
(1) weighing 50g of polyvinyl alcohol (PVA), slowly adding the PVA into 200mL of deionized water, and stirring for 6 hours until the PVA is completely dissolved in the deionized water to prepare the adhesive; weighing 0.5g of dried 8000-mesh crystalline flake graphite, adding the dried crystalline flake graphite into the prepared adhesive, and continuously stirring to uniformly mix graphite powder into the adhesive;
(2) starting the machine, moving the double-roller columns 12 and 13 into the roller 14 through the lifting module 2, and rotating the double-roller columns 12 and 13 through the rotating speed adjusting window 6; slowly adding an adhesive containing graphite powder into the roller 14 from the feeding hole 8, after the materials are uniformly spread on the surfaces of the double-roller columns 12 and 13 and the inner wall of the roller 14, adjusting the rotating speed of the double-roller columns 12 and 13 to 80rpm/min and the temperature to 25 ℃, and starting stripping;
(3) after the completion, the materials are gradually scraped from the upper discharge port 9, and then the double-roller columns 12 and 13 and the roller 14 are washed by deionized water, and the residual materials are collected from the lower discharge port 10. And mixing the materials collected twice with 1000mL of deionized water, standing the obtained mixed solution for 24h, filtering out bottom precipitates, carrying out ultrasonic treatment on the upper-layer dispersion liquid for 5min, filtering, carrying out centrifugal washing with 1000mL of deionized water for three times, and drying to obtain the graphene.
The morphology of the 8000-mesh crystalline flake graphite used in the example and the prepared graphene is characterized by a scanning electron microscope, and the result is shown in fig. 3, wherein the crystalline flake graphite is in a thick sheet shape and is mainly caused by multilayer stacking; the graphene product prepared in this example exhibited a typical two-dimensional sheet structure, indicating a smooth and three-dimensional wrinkled structure.
XRD tests were carried out on the 8000 mesh scale graphite used in this example and the samples obtained by exfoliation for various times, and the results are shown in FIG. 4. It can be obviously seen that the 8000-mesh crystalline flake graphite has a sharp diffraction peak at about 26 degrees, and the peak corresponds to the (002) crystal face of the graphite, which shows that the three-dimensional layered structure of the raw material is obvious; and with the prolonging of the stripping time, the diffraction characteristic peak intensity of the graphite begins to weaken, and particularly, the diffraction peak of a sample stripped by 7d disappears, which shows that the three-dimensional layered structure is converted into a two-dimensional sheet structure, and the structure characteristics of the graphene are met.
The results of the Raman test on the 8000 mesh scale graphite used in this example and the samples obtained by exfoliation for various times are shown in fig. 5. Generally, the number of layers of the sample can be simply judged according to the peak position and the peak intensity of the 3D peak, and after the result is analyzed, the 2D peak of the exfoliated graphite is shifted to the left, the peak intensity is enhanced relative to the G peak, and particularly the sample is stripped for 7D, which indicates that the number of layers of the exfoliated graphite is reduced.
TABLE 1
Dispersing the micro-stripped sample of 7d in N-methyl pyrrolidone to prepare a very dilute solution, dripping the solution on mica, and drying the mica in an oven. The theoretical thickness of a single-layer graphene sheet is 0.35nm, but due to factors such as chemical substrates and interlayer functional groups, the actual thickness is greater than 0.35 nm. According to the height of the graphene product shown in fig. 6, it can be known that the thickness of the exfoliated graphite flakes is 1.5-2.0nm after 7 days, so that few layers of graphene can be obtained, and the number of layers is about 3-5.
Example 3
Example 3 differs from example 2 in that:
weigh 0.5g of dried 8000 mesh flake graphite and 80g of sucrose, and mix well with a glass rod.
Starting the machine, setting the stripping temperature in the control module 1 at 160 ℃, and rotating the twin-roll columns 12, 13; and slowly adding the sucrose containing graphite powder into the roller 14 from the feeding hole 8, and after the materials are melted and uniformly spread on the surfaces of the double-roller columns 12 and 13 and the inner wall of the roller 14, adjusting the rotating speed of the double-roller columns to 80rpm/min and starting stripping.
The materials are gradually scraped from the upper discharge port 9, the double-roller column and the roller are washed by deionized water, and the residual materials are collected from the lower discharge port 10. And mixing the materials collected twice with 1000mL of deionized water, standing the obtained mixed solution for 24h, filtering out bottom precipitates, carrying out ultrasonic treatment on the upper-layer dispersion liquid for 5min, filtering, carrying out centrifugal washing with 1000mL of deionized water for three times, and drying to obtain the graphene.
Example 4
Example 4 differs from example 2 in that:
0.5g of dried expanded graphite and 80g of sucrose were weighed, and mixed well with a glass rod.
Starting the machine, setting the stripping temperature at 160 ℃ in the control module 1, and rotating the twin-roll columns 12, 13; slowly adding sucrose containing graphite powder into the roller 14 from the feeding hole 8, after the materials are melted and uniformly spread on the surfaces of the double-roller columns 12 and 13 and the inner wall of the roller 14, adjusting the rotating speed of the double-roller columns 12 and 13 to 80rpm/min, and starting to strip.
The materials are gradually scraped from the upper discharging port 9, and then the double-roller columns 12 and 13 and the roller 14 are washed by deionized water, and the residual materials are collected from the lower discharging port 10. And mixing the materials collected twice with 1000ml of deionized water, standing the obtained mixed solution for 24h, filtering out bottom precipitates, carrying out ultrasonic treatment on the upper-layer dispersion liquid for 5min, filtering, washing with 1000ml of deionized water for three times, and drying to obtain the graphene.
Example 5
Example 5 differs from example 2 in that:
weighing 50g of polyvinyl alcohol (PVA), slowly adding the PVA into 200ml of deionized water, and stirring for 6 hours until the PVA is completely dissolved in the deionized water to prepare the adhesive; 0.5g of dried expanded graphite is weighed and added into the prepared adhesive, and the mixture is continuously stirred to enable graphite powder to be uniformly mixed into the adhesive.
Starting the machine to rotate the twin roll columns 12, 13; slowly adding an adhesive containing graphite powder into the roller 14 from the feeding hole 8, after the materials are uniformly spread on the surfaces of the double-roller columns 12 and 13 and the inner wall of the roller 14, adjusting the rotating speed of the double-roller columns 12 and 13 to 80rpm/min and the temperature to 25 ℃, and starting stripping.
The materials are gradually scraped from the upper discharging port 9, and then the double-roller columns 12 and 13 and the roller 14 are washed by deionized water, and the residual materials are collected from the lower discharging port 10. And mixing the materials collected twice with 1000ml of deionized water, standing the obtained mixed solution for 24h, filtering out bottom precipitates, carrying out ultrasonic treatment on the upper-layer dispersion liquid for 5min, filtering, washing with 1000ml of deionized water for three times, and drying to obtain the graphene.
The above description is only a preferred embodiment of the present invention, and therefore should not be taken as limiting the scope of the invention, which is defined by the appended claims and their equivalents.
Claims (9)
1. The utility model provides a device of preparation graphite alkene strips in succession which characterized in that: the device comprises a stripping module, a lifting module, a driving module and a control module;
the peeling module comprises a roller, the roller is provided with a heater, and a first roller column and a second roller column are arranged in the roller; the first roller and the second roller are arranged side by side in a gap of 0.3-0.4 cm, and the gap between the outer walls of the first roller and the second roller and the inner wall of the roller is 0.3-0.4 cm; the outer wall of the first roller is provided with threads with the thread pitch of 0.2-0.3 cm and the depth of 0.2-0.3 cm, and the outer wall of the second roller is smooth;
the driving module is connected with the first roller and the second roller;
the lifting module is used for controlling the heights of the first roller and the second roller;
the control module is connected with the stripping module, the lifting module and the driving module and used for supplying power and controlling the temperature of the roller and the rotating speed and the height of the first roller and the second roller.
2. The device for preparing graphene by continuous stripping according to claim 1, wherein: the roller is provided with a feed inlet, an upper discharge port and a lower discharge port, the feed inlet and the upper discharge port are located on the upper portion of the roller on one side where the first roller is located, and the lower discharge port is located on the lower portion of the roller on one side where the second roller is located.
3. The device for preparing graphene by continuous stripping according to claim 2, wherein: the cross section of the upper discharge port is square, and the cross section of the lower discharge port is circular.
4. The device for preparing graphene by continuous stripping according to claim 1, wherein: the gap between the outer walls of the first roller and the second roller and the inner wall of the roller is 0.4cm, the outer wall of the first roller is provided with threads with the thread pitch of 0.2cm and the depth of 0.2cm, and the gap between the first roller and the second roller is 0.3 cm.
5. The device for preparing graphene by continuous stripping according to claim 1, wherein: the control module comprises a control panel, and a power switch, a temperature adjusting window and a rotating speed adjusting window are arranged on the control panel.
6. A method for preparing graphene by continuous stripping is characterized by comprising the following steps: the method adopts the device as claimed in any one of claims 1 to 5, and comprises the following specific steps:
(1) mixing graphite powder and an adhesive in a ratio of 0.1-1: mixing the components in a mass ratio of 10-200 to obtain an adhesive containing graphite powder; the adhesive is one of polyvinyl alcohol, honey, isopropanol, sucrose and maltose, and the viscosity of the adhesive is controlled within the range of 600-1000 mPa.s.
(2) Adding an adhesive containing graphite powder into a roller from a feed inlet of the device for stripping for 7d, wherein the stripping temperature is 25-200 ℃, and the stripping rotating speed is 100-200 rpm;
(3) the materials on the outer wall of the first roller are collected through the upper discharging hole, the stripping device is washed by deionized water, the residual materials are collected through the lower discharging hole, and the materials collected twice are mixed and then purified to obtain a graphene product.
7. The device for preparing graphene by continuous stripping according to claim 6, wherein: the specification of the graphite powder in the step (1) is 50-8000 meshes.
8. The device for preparing graphene by continuous stripping according to claim 6, wherein: when the adhesive is polyvinyl alcohol, honey and isopropanol, the stripping temperature is 20-25 ℃; when the adhesive is cane sugar or maltose, the peeling temperature is 150-200 ℃.
9. The device for preparing graphene by continuous stripping according to claim 6, wherein: the purification treatment in the step (3) comprises the following steps: and standing the mixed material, carrying out ultrasonic treatment on the upper-layer dispersion liquid with the power of 1000-1100W and the frequency of 20-25 kHz for 5-10 min, and then filtering, centrifuging and drying.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115818630A (en) * | 2022-11-21 | 2023-03-21 | 中国铝业股份有限公司 | Graphene stripping device and graphene production system |
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| CN204281322U (en) * | 2014-10-23 | 2015-04-22 | 常州二维碳素科技有限公司 | A kind of stripping off device |
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