CN114314572A - High-temperature reaction tube for preparing graphene by electrifying carbon powder - Google Patents
High-temperature reaction tube for preparing graphene by electrifying carbon powder Download PDFInfo
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- CN114314572A CN114314572A CN202011075836.XA CN202011075836A CN114314572A CN 114314572 A CN114314572 A CN 114314572A CN 202011075836 A CN202011075836 A CN 202011075836A CN 114314572 A CN114314572 A CN 114314572A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 85
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 57
- 238000006243 chemical reaction Methods 0.000 title claims abstract description 55
- 229920000642 polymer Polymers 0.000 claims abstract description 29
- 229910052751 metal Inorganic materials 0.000 claims abstract description 15
- 239000002184 metal Substances 0.000 claims abstract description 15
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 27
- 229910052802 copper Inorganic materials 0.000 claims description 27
- 239000010949 copper Substances 0.000 claims description 27
- -1 Polytetrafluoroethylene Polymers 0.000 claims description 16
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 15
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 15
- 239000004696 Poly ether ether ketone Substances 0.000 claims description 8
- 239000004693 Polybenzimidazole Substances 0.000 claims description 8
- 239000004642 Polyimide Substances 0.000 claims description 8
- 229920000265 Polyparaphenylene Polymers 0.000 claims description 8
- 229920002480 polybenzimidazole Polymers 0.000 claims description 8
- 229920002530 polyetherether ketone Polymers 0.000 claims description 8
- 229920001721 polyimide Polymers 0.000 claims description 8
- 229910052782 aluminium Inorganic materials 0.000 claims description 4
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 4
- 229920002312 polyamide-imide Polymers 0.000 claims description 4
- 229910001220 stainless steel Inorganic materials 0.000 claims description 4
- 239000010935 stainless steel Substances 0.000 claims description 4
- 238000001704 evaporation Methods 0.000 abstract description 21
- 238000000034 method Methods 0.000 abstract description 12
- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 7
- 239000000843 powder Substances 0.000 description 16
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 11
- 230000008020 evaporation Effects 0.000 description 7
- 238000001237 Raman spectrum Methods 0.000 description 6
- 239000000463 material Substances 0.000 description 6
- 239000010453 quartz Substances 0.000 description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 6
- RHZUVFJBSILHOK-UHFFFAOYSA-N anthracen-1-ylmethanolate Chemical compound C1=CC=C2C=C3C(C[O-])=CC=CC3=CC2=C1 RHZUVFJBSILHOK-UHFFFAOYSA-N 0.000 description 4
- 239000003830 anthracite Substances 0.000 description 4
- 239000010410 layer Substances 0.000 description 4
- 238000001878 scanning electron micrograph Methods 0.000 description 4
- 238000001069 Raman spectroscopy Methods 0.000 description 3
- 239000003610 charcoal Substances 0.000 description 3
- 239000000571 coke Substances 0.000 description 3
- 238000010924 continuous production Methods 0.000 description 3
- 229910002804 graphite Inorganic materials 0.000 description 3
- 239000010439 graphite Substances 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000002086 nanomaterial Substances 0.000 description 3
- 238000010923 batch production Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 238000001000 micrograph Methods 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 230000036632 reaction speed Effects 0.000 description 2
- 238000005299 abrasion Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 239000006229 carbon black Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000004313 glare Effects 0.000 description 1
- 230000017525 heat dissipation Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000013081 microcrystal Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 238000013341 scale-up Methods 0.000 description 1
- 238000004626 scanning electron microscopy Methods 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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Abstract
In order to reduce the equipment cost for preparing graphene by an electric flash method, the invention provides a high-temperature reaction tube for preparing graphene by electrifying carbon powder, which is a double-layer tube formed by tightly combining a polymer inner tube and a metal outer tube. The double-layer tube can be repeatedly used for thousands of times, effectively reduces the cost of preparing graphene by an electric flash evaporation method, and provides a new process technology for large-scale production of graphene.
Description
Technical Field
The invention belongs to the field of nano material preparation, and particularly relates to a high-temperature reaction tube for preparing graphene by electrifying carbon powder.
Background
Graphene is a two-dimensional nano material composed of single-layer honeycomb-shaped carbon atoms, is the thinnest, lightest, strongest and hardest material, has excellent electric conduction and heat conduction performance, and is called as the king of materials. The current large-scale production of graphene is primarily a graphite redox process. In view of the problems of complex process technology, waste liquid treatment and the like, the production cost of the graphene is very high, the price of the graphene powder in the market is high, and the large-scale application of the graphene is limited.
WO2020/051000 (Flash Joule Heating Synthesis Method and Compositions theory) discloses a Method for preparing graphene by electric power through a Joule Heating Flash evaporation Method, wherein carbon powder such as carbon black, coke or anthracite is put in a quartz tube, large current is applied for less than 1 second, the temperature is as high as about 3000 ℃, and the carbon powder is instantly changed into graphene. For the estimation of the power cost, only 2 degrees of electricity are needed for producing 1 kg of graphene, and the power cost is as low as 1 yuan. However, only about 1 g of graphene can be prepared by one-time electric flash evaporation, and a quartz tube with the cost of 1 yuan is fragile and cannot be used due to the 3000 ℃ high temperature generated by the reaction. Thus, the production cost of the electric flash evaporation method is increased dramatically to about 1000 yuan per kilogram of graphene, and the cost advantage is basically lost.
In order to realize low-cost large-scale production, a high-temperature resistant reaction tube which replaces a quartz tube must be found in the electric flash evaporation method, the high-temperature resistant reaction tube can be repeatedly used, and the cost of reaction equipment is reduced.
Disclosure of Invention
The invention aims to solve the problem of high temperature resistance of a reaction tube for preparing graphene by an electric flash evaporation method, and provides a high-temperature reaction tube for preparing graphene by electrifying carbon powder.
In order to achieve the purpose, the invention adopts the technical scheme that:
a high-temperature reaction tube for preparing graphene by electrifying carbon powder is a double-layer tube formed by tightly combining a polymer inner tube and a metal outer tube.
Further, the polymer inner tube is made of Polytetrafluoroethylene (PTFE), polyparaphenylene (PPL), Polybenzimidazole (PBI), Polyetheretherketone (PEEK), Polyimide (PI), or Polyamideimide (PAI).
Further, the inner diameter of the polymer inner tube is 10 to 200 mm.
Further, the wall of the polymer inner pipe is 0.1 to 50 mm.
Further, the metal outer tube is made of copper, aluminum or stainless steel.
Further, the pipe wall of the metal outer pipe is 0.5-100 mm.
The invention has the beneficial effects that:
(1) although the polymer inner tube is usually used in a high-temperature environment of 200 ℃, the polymer inner tube can bear the impact of ultra-high temperature of 3000 ℃ for 1 second, and can be used for many times, thereby replacing inorganic high-temperature materials with high brittleness, such as a quartz tube.
(2) The polymer inner tube is electrically insulated, and current can only pass through carbon powder in the tube, so that the carbon powder is heated to 3000 ℃ instantly, and the smooth reaction of graphene prepared by an electric flash method in the polymer inner tube is ensured.
(3) The metal outer pipe can improve the strength of the polymer inner pipe with higher flexibility, can also quickly absorb and dissipate heat generated in the reaction, and effectively protects the polymer inner pipe in the aspects of strength and heat dissipation.
Compared with the electric flash evaporation process using the quartz tube, the invention has the following advantages: (1) the cost for preparing the graphene is greatly reduced. The high-temperature reaction tube can be used for thousands of times, the equipment cost for preparing the graphene by the electric flash evaporation method is reduced to less than 1 yuan, and the total preparation cost is reduced to several yuan per kilogram. (2) The process scale-up is easy to perform. The inner diameter of the high-temperature reaction tube can be larger, and hundreds of grams of carbon powder is filled each time, so that the high-temperature reaction tube is suitable for large-scale production.
Drawings
FIG. 1 is a diagram of an apparatus for preparing graphene by an electric flash method according to the present invention.
FIG. 2 is a scanning electron micrograph of graphene prepared according to the present invention.
Fig. 3 is a raman spectrum of graphene prepared according to the present invention.
Detailed Description
The invention is further described below with reference to the figures and examples.
The experimental methods described in the following examples are all conventional methods unless otherwise specified; the starting materials and materials used, if not specifically required, are commercially available. The power supply used was a 100 kilowatt dc power supply (maximum voltage 200V and maximum current 500A).
Example 1
As shown in fig. 1, the high temperature reaction tube for preparing graphene by electrifying carbon powder in this embodiment includes a polymer inner tube 1 and a metal outer tube 2 which are tightly combined, reactant carbon powder 3 is placed in the middle of the inner tube, two copper plugs 4 and 5 are respectively arranged at two ends of the inner tube to block the carbon powder in the middle, the two copper plugs are respectively connected with copper electrodes 6 and 7, and the copper electrodes are further connected with a positive electrode 9 and a negative electrode 10 of a direct current power supply 8.
The polymer inner pipe is made of Polytetrafluoroethylene (PTFE), the inner diameter of the polymer inner pipe is 10 mm, and the pipe wall is 5 mm; the metal outer pipe is a copper outer pipe, the inner diameter of the metal outer pipe is 20 mm, and the pipe wall of the metal outer pipe is 5 mm. Therefore, the polytetrafluoroethylene inner tube and the copper outer tube are tightly sleeved together to form the high-temperature reaction tube for preparing the graphene by the electric flash evaporation method.
The using method of the device comprises the following steps: one end of the reaction tube is plugged with a copper plug, 0.5 g of conductive carbon black is poured, the other end of the reaction tube is plugged with the copper plug, and the two copper plugs are compressed, so that the conductive carbon black is kept in the middle of the reaction tube. The outer sides of the copper plugs were each pressed with a copper electrode and the resistance was measured to be about 1 ohm.
The whole reaction tube is placed in a vacuum box, a discharge circuit is connected, and the vacuum is pumped to 0.1 atmosphere. The power supply was turned on, the voltage was selected to be 200 volts, and the discharge was 200 milliseconds, causing glare from the copper plug. Cutting off the power supply, putting gas into the vacuum box, opening the vacuum box, taking out the reaction tube, and ensuring the temperature of the copper tube to be about 45 ℃. The product was poured out of the tube and ground to a black powder. Scanning electron microscopy of these black powders (fig. 2) revealed that a lamellar structure had been produced. The black powders were examined by laser raman spectroscopy to obtain a raman spectrum (fig. 3), in which the G peak indicates the vibration of the graphite sheet, the D peak indicates the size and defect of the graphene sheet, and the 2D peak indicates the number of layers of the graphene. The black powder can be analyzed from a Raman spectrum, and is a graphene nano material with less than 5 layers.
At the moment, the polymer inner tube of the reaction tube is completely free from any damage, and the electric flash reaction is carried out for multiple times; after 100 times of reaction, the inner tube of the polymer has certain abrasion; at 2000 times, the inner diameter of the polymer inner tube increased by about 0.2 mm; at 10000 times, the inner diameter of the polymer inner tube increased by about 1 mm. Therefore, compared with a quartz tube with larger brittleness, the polymer inner tube and the high-temperature reaction tube of the metal outer tube can be repeatedly used, and the equipment cost for preparing graphene by an electric flash evaporation method is greatly reduced.
Example 2
The inner polymer tube of the reactor was fabricated using polyparaphenylene (PPL), Polybenzimidazole (PBI), Polyetheretherketone (PEEK), Polyimide (PI) or Polyamideimide (PAI) using the reaction apparatus of example 1, and the inner diameter and wall thickness thereof were the same as those of the inner polytetrafluoroethylene tube of example 1, and the outer copper tube was also the same as those of example 1, and 0.5 g of conductive carbon black was charged into each of the fabricated reaction tubes to perform an electric flash evaporation reaction. The obtained powder was tested to obtain a scanning electron micrograph and a raman spectroscopy, which are substantially the same as those of example 1, and it was confirmed that each of the graphene materials having 5 or less layers was obtained.
The electric flash reaction was carried out a plurality of times, and the inner diameter of polyparaphenylene (PPL), Polybenzimidazole (PBI), Polyetheretherketone (PEEK), Polyimide (PI) and Polyamideimide (PAI) was worn to 1 mm after 20000 times, 25000 times, 18000 times, 22000 times and 26000 times, respectively. Therefore, the high-temperature polymers can also be used as a polymer inner tube material for preparing graphene by an electric flash evaporation method.
Example 3
The inner diameters of the polytetrafluoroethylene inner pipes in the embodiment 1 are respectively selected to be 8 mm, 10 mm, 20 mm, 100 mm, 200 mm and 250 mm, and the wall thickness of the inner pipe is 5 mm; the inner diameters of the copper outer tubes are 18 mm, 20 mm, 30 mm, 110 mm, 210 mm and 260 mm respectively, and the wall thickness is 5 mm, so that 6 types of reactors for preparing graphene by electric flash evaporation are manufactured respectively.
When the inner diameter of the polytetrafluoroethylene inner tube is 8 mm, only 0.2 g of conductive carbon black can be filled each time, the production speed is very low, and the polytetrafluoroethylene inner tube is not suitable for large-scale production.
When the inner diameter of the inner tube is 10 mm, 20 mm, 100 mm and 200 mm, 0.5 g, 2.0 g, 50 g and 200 g of conductive carbon black can be filled in each time, the resistance is 1 ohm, 0.5 ohm, 0.1 ohm and 0.05 ohm respectively, the electric flash evaporation reaction can be normally carried out, the scanning electron microscope image and the Raman spectrum image of the obtained black powder are the same as or similar to those of the example 1, and the normal reaction and the generation of graphene are proved. It can be seen that the reaction tube for preparing graphene by the electric flash evaporation method can be used for large-scale production.
When the inner diameter of the polymer inner tube is 250 mm, 320 g of conductive carbon black can be filled in each time, the electric flash reaction can normally discharge, but strong light can not flash, and the scanning electron microscope image and the Raman spectrum image of the obtained black powder show that the black powder is mainly graphite microcrystal. Therefore, the inner diameter of the inner tube of 250 mm is too large to be used for preparing graphene by an electric flash evaporation method.
Therefore, the most preferred inner diameter of the polymer inner tube is 10 to 200 mm. Too small an inner diameter is not conducive to large-scale production, and too large a diameter does not yield graphene powder.
Example 4
The inner diameter of the polytetrafluoroethylene inner tube in example 1 was changed to 10 mm, and the tube wall was changed to 0.05, 0.1, 1, 5, 10, 30, 50, 70 mm, respectively; the inner diameters of the copper outer tubes are 10.1 mm, 10.2 mm, 12 mm, 20 mm, 30 mm, 70 mm, 110 mm and 150 mm, and the tube walls are 5 mm, so that 8 high-temperature reaction tubes for preparing graphene by using an electric flash evaporation method are respectively manufactured. 0.5 g of conductive carbon black is put into the reactor each time, and the graphene is prepared by electrifying.
When the wall of the inner tube is 0.05 mm, the inner tube is worn out after about 100 times of reaction, so that the carbon powder and the copper outer tube are conductive and cannot be normally used.
When the pipe wall of the inner pipe is 0.1 mm, 1 mm, 5 mm, 10 mm, 30 mm or 50 mm, the reaction can be normally carried out for more than 10000 times, and graphene can be normally produced.
When the pipe wall of the inner pipe is 70 mm, the heat generated by the reaction cannot be normally conducted to the copper outer pipe, so that the temperature of the polytetrafluoroethylene inner pipe is increased and softened, the reaction speed is forced to be slowed down, and the continuous batch production of graphene is not suitable.
This indicates that the optimum thickness of the wall of the inner polymer tube is 0.1 to 50 mm, and the reaction tube can be reused for a long time, and can conduct heat rapidly to perform continuous production at a high speed.
Example 5
The copper outer tube in example 1 was changed to aluminum or stainless steel, respectively, and the dimensions were not changed, so as to fabricate two high-temperature reaction tubes for preparing graphene by electric flash evaporation. 0.5 g of conductive carbon black is added each time, and the graphene is prepared by electric flash evaporation. The scanning electron micrograph and the raman spectrum of the obtained black powder were identical to those of example 1.
The continuous production can be carried out by using the two devices for more than 10000 times. Thus, the metal outer tube may be made of copper, aluminum or stainless steel.
Example 6
The inner diameter of the polytetrafluoroethylene inner tube in example 1 was set to 10 mm, and the tube wall was set to 5 mm; the inner diameter of the copper outer tube is 20 mm, the tube wall is changed into 0.2 mm, 0.5 mm, 1 mm, 5 mm, 50 mm, 100 mm and 150 mm, and 7 high-temperature tubes for preparing graphene by using the electric flash evaporation method are respectively manufactured. 0.5 g of conductive carbon black is put into the reactor each time, and the graphene is prepared by electrifying.
When the wall of the copper pipe is 0.2 mm, the inner pipe is softened and deformed after 100 times of reaction, and cannot be used normally.
When the pipe wall of the copper pipe is 0.5 mm, 1 mm, 5 mm, 50 mm and 100 mm, the reaction can be normally carried out for more than 10000 times, and graphene can be normally produced.
When the wall of the copper pipe is 150 mm, heat generated by reaction is gathered in the copper outer pipe and cannot be normally conducted to air, so that the temperature of the polytetrafluoroethylene inner pipe is increased and softened, the reaction speed is forced to be slowed down, and the continuous batch production of graphene is not suitable.
This indicates that the optimal thickness of the wall of the metal outer tube is 0.5 to 100 mm, and the reaction tube can be reused for a long time, and can conduct heat rapidly to perform continuous production at a high speed.
Example 7
Using the reaction apparatus of example 1, 0.4 g of 800 mesh coke, anthracite and charcoal powder and 0.1 g of conductive carbon black were uniformly mixed, respectively, to obtain three kinds of carbon powders. The three kinds of carbon powder are respectively filled into a reaction tube, and the resistances of the coke powder, the anthracite powder and the charcoal powder are respectively 3.2 ohm, 3.5 ohm and 4.1 ohm. The discharge was performed according to the energization procedure of example 1, and the flash was intense. The scanning electron micrograph and the Raman spectrogram of the product after the reaction are similar to those of the conductive carbon black. The high-temperature reaction tube is suitable for preparing graphene from coke, anthracite and charcoal powder, and is also suitable for preparing graphene by most types of carbon powder electric flash evaporation methods.
The above description is only an embodiment of the present invention, and not intended to limit the scope of the present invention, and all modifications of equivalent structures and equivalent processes, or direct or indirect applications in other related fields, which are made by the contents of the present specification, are included in the scope of the present invention.
Claims (6)
1. A high-temperature reaction tube for preparing graphene by electrifying carbon powder is characterized in that: it is a double-layer tube formed by tightly combining a polymer inner tube and a metal outer tube.
2. The high-temperature reaction tube for preparing graphene by electrifying carbon powder according to claim 1, which is characterized in that: the polymer inner tube is made of Polytetrafluoroethylene (PTFE), polyparaphenylene (PPL), Polybenzimidazole (PBI), Polyetheretherketone (PEEK), Polyimide (PI) or Polyamideimide (PAI).
3. The high-temperature reaction tube for preparing graphene by electrifying carbon powder according to claim 1, which is characterized in that: the inner diameter of the polymer inner tube is 10 to 200 mm.
4. The high-temperature reaction tube for preparing graphene by electrifying carbon powder according to claim 1, which is characterized in that: the wall of the polymer inner pipe is 0.1 to 50 mm.
5. The high-temperature reaction tube for preparing graphene by electrifying carbon powder according to claim 1, which is characterized in that: the metal outer pipe is made of copper, aluminum or stainless steel.
6. The high-temperature reaction tube for preparing graphene by electrifying carbon powder according to claim 1, which is characterized in that: the pipe wall of the metal outer pipe is 0.5-100 mm.
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Application publication date: 20220412 |