CN213356969U - 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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Abstract
In order to reduce the equipment cost of electricity flash process preparation graphite alkene, the utility model provides a carbon dust circular telegram preparation graphite alkene's high temperature reaction tube, it is the double-layer tube of combining closely by polymer inner tube and metal outer tube and forming. 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 utility model belongs to nano-material preparation field, concretely relates to carbon dust circular telegram preparation graphite alkene's high temperature reaction pipe.
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 utility model aims at solving the high temperature resistant problem of reaction tube of electricity flashing method preparation graphite alkene, provide a carbon dust circular telegram preparation graphite alkene's high temperature reaction tube.
In order to achieve the above object, the utility model adopts the following technical scheme:
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 beneficial effects of the utility model reside in that:
(1) the polymer inner tube of the utility model is commonly used in the high temperature environment of 200 ℃, but can bear the impact of 1 second ultra-high temperature of 3000 ℃ and can be used for a plurality of times, thereby replacing the inorganic high-temperature material with higher brittleness like quartz tube.
(2) The utility model discloses a polymer inner tube is electrical insulation, and the electric current can only be followed intraductal carbon dust and passed through to heat the carbon dust to 3000 ℃ in the twinkling of an eye, just so guaranteed that the electricity dodges the evaporation method and prepare graphite alkene and react smoothly at the polymer inner tube.
(3) The utility model discloses a metal outer tube both can improve the intensity of the higher polymer inner tube of flexibility, also can be fast with the heat absorption and the distribution away that produce during the reaction, effectively protected the polymer inner tube in two aspects of intensity and heat dissipation.
The utility model discloses compare with the electric flash process who uses the quartz capsule, have following advantage: (1) the cost for preparing the graphene is greatly reduced. The high-temperature reaction tube of the utility model 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 evaporation method of the present invention.
Fig. 2 is a scanning electron microscope image of the graphene preparation of the present invention.
Fig. 3 is a raman spectrogram of graphene prepared by the present invention.
Detailed Description
The invention is further described with reference to the following 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. This shows that the high temperature reaction tube of the utility model 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 is only the embodiment of the present invention, not limiting the scope of the present invention, all of which utilize the equivalent structure or equivalent flow transformation made by the content of the present invention, or directly or indirectly applied to other related technical fields, and all included in the same way in the protection scope of the present invention.
Claims (6)
1. A high-temperature reaction tube for preparing graphene by electrifying carbon powder is characterized in that: the double-layer tube is formed by tightly combining a polymer inner tube and a metal outer tube, wherein reactant carbon powder is placed in the middle of the inner tube, two copper plugs are respectively arranged at two ends of the inner tube to plug the carbon powder in the middle, the two copper plugs are respectively connected with copper electrodes, and the copper electrodes are connected with the positive electrode and the negative electrode of a direct-current power supply.
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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Effective date of registration: 20221227 Address after: 030001 room 1104, Baocheng apartment, Nanhai street, Yingze District, Taiyuan City, Shanxi Province Patentee after: Lv Haigang Patentee after: Taiyuan Saiyin New Material Technology Co.,Ltd. Address before: 030001 room 1104, Baocheng apartment, Nanhai street, Yingze District, Taiyuan City, Shanxi Province Patentee before: Lv Haigang Patentee before: Beijing saiyintuopu Technology Co.,Ltd. |