A method for efficiently removing oxygen from carbon materials
By using the method of pressurization, heating and depressurization cycles, the oxygen element in the carbon material can be efficiently removed at low temperature, which solves the problems of poor universality and limited deoxidation effect in the existing technology, realizes efficient deoxidation of porous carbon materials, and avoids the damage to the structure caused by high-temperature treatment.
Patent Information
- Application Number
- CN202211633750.3
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2022-12-19
- Publication Date
- 2025-09-30
- Estimated Expiration
- 2042-12-19
AI Technical Summary
Existing technologies have poor universality in removing oxygen from carbon materials. High-temperature treatment may cause structural changes in the carbon materials, and reducing gases are difficult to fully diffuse into the interior of the material, resulting in limited deoxidation effects.
The deoxidation reduction reaction is carried out at 0.05-10MPa and 20-200°C by adopting the method of pressurization, heating and depressurization cycles. By adjusting the reducing gas partial pressure and the number of cycles, it is ensured that the reducing gas fully contacts and diffuses with the material, thereby reducing the reaction activation energy. It is suitable for a variety of carbon materials.
It achieves efficient deoxidation at lower temperatures, avoids structural changes in carbon materials, is applicable to porous carbon materials, improves deoxidation effect and efficiency, and reduces costs.
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Figure CN118221098B_ABST
Abstract
Description
Technical Field
[0001] The present invention relates to the technical field of carbon materials, and in particular to a method for efficiently removing oxygen from carbon materials. Background Art
[0002] Carbon materials are a class of substances primarily composed of the element carbon, including activated carbon, carbon fibers, carbon nanotubes, graphene, capacitor carbon, and various artificial graphite materials. Carbon materials play an irreplaceable role in various fields due to their adsorption, conductivity, and strength properties. These properties of carbon materials primarily derive from their carbon content. Except for certain specialized applications where carbon materials require specific element doping to regulate their physical and chemical properties, the presence of elements other than carbon is generally undesirable in carbon materials.
[0003] Oxygen is the most common impurity in various carbon materials, with a content as high as 15%. This is due to the use of oxygen-rich raw materials (such as coconut shells and straw used to make activated carbon) during the preparation process, as well as the oxidation of the materials. In applications, oxygen often has an adverse effect on the application of carbon materials. For example, the oxygen in activated carbon used in supercapacitor electrodes (capacitor carbon / capacitor activated carbon) will react with the electrolyte, resulting in a decrease in device stability and lifespan. For another example, activated carbon used as catalyst carriers or in the medical field will interfere with the reaction or adsorption process due to the presence of impurity oxygen. Therefore, removing oxygen from carbon materials is of great significance to the application of carbon materials.
[0004] The reduction process of graphite oxide or graphene oxide involves the removal of oxygen, but the reducing agents currently used are expensive and environmentally polluting. Alternatively, the carbon material can be treated in an inert atmosphere to reduce the oxygen in the material to water. Previously reported methods often rely on high-temperature treatment to enable the deoxygenation reaction or improve its efficiency. For example, Du et al. (CN109592681A) calcined activated carbon materials under a reducing atmosphere (ammonia) to remove oxygen elements. In this method, the reducing gas is difficult to fully diffuse into the surface and pores of the material, and the deoxidation effect is limited. The material is dependent on being heated, and the reducing gas used is ammonia (NH3), which is expensive and highly corrosive, and is not suitable for large-scale preparation. Zhang et al. (CN106082210A) removed oxygen elements by high-temperature treatment (650-1200°C) of carbon materials, but this method is not applicable to some temperature-sensitive carbon materials. Chen et al. (CN110482548A) removed oxygen from supercapacitor activated carbon by heating it in a fluidized bed operated in a hydrogen-nitrogen mixed atmosphere. Although the contact form between the material and the reducing gas is improved, for porous carbon materials such as activated carbon, the reducing gas is still difficult to enter the pores of the material, and the reduction effect is limited. In addition, the fluidized state of the material is difficult to control, the reducing gas consumption is large, and the operating cost is high.
[0005] In summary, the existing methods for removing oxygen from carbon materials have the following shortcomings: 1) They rely on high-temperature treatment to achieve deoxidation reaction, but the structure of the carbon material may change at high temperature, and high-temperature treatment is not applicable to some temperature-sensitive carbon materials; 2) The reducing gas only contacts the material to be deoxidized by flowing or blowing, and the interaction force between the material and the reducing gas molecules is weak and it is not easy to diffuse into the interior of the material, especially for some porous carbon materials. The deoxidation effect is limited, and the water generated after this normal pressure reaction deoxidation is not easy to separate from the carbon material. Summary of the Invention
[0006] The purpose of the present invention is to solve the problem that the methods for removing oxygen from carbon materials in the prior art have poor universality. In response to the above problems, the present invention provides a method for efficiently removing oxygen from carbon materials. The method has excellent universality. By pressurizing the deoxidation environment, the activation energy of the reaction is reduced, and the deoxidation of the carbon material can be achieved at a relatively low temperature, avoiding the transformation of the temperature-sensitive carbon material structure caused by high temperature. Moreover, the reducing gas can fully contact with the material and diffuse into the interior of the material, and has an excellent deoxidation effect on porous carbon materials. In addition, the reducing gas partial pressure can be adjusted according to the structure of the material and different oxygen contents, and the deoxidation reaction efficiency is high, the effect is good, and the cost is low.
[0007] In order to achieve the above object, the present invention adopts the following technical solutions:
[0008] A method for efficiently removing oxygen from carbon materials comprises the following steps:
[0009] Pressurization and heating: The carbon material is subjected to deoxidation reduction reaction in a reducing gas atmosphere at 0.05-10 MPa and 20-200°C;
[0010] Depressurization: performing a temperature and pressure reduction treatment on the carbon material after the deoxidation reduction reaction is completed;
[0011] After the steps of pressurizing, heating and reducing pressure are cycled 0 to 10 times, the pressure is released and the by-products are discharged, thereby obtaining the carbon material after the oxygen element is removed.
[0012] In the method for efficiently removing oxygen from carbon materials provided by the present invention, the number of cycles of pressurization, temperature increase, and pressure reduction can be adjusted based on the actual deoxidation effect to meet the oxygen content standard of the carbon material. For example, the present invention recommends that the number of repetitions of pressurization, temperature increase, and pressure reduction be 2 to 4.
[0013] This method can achieve good deoxidation efficiency at a relatively low temperature, and the process parameter control is relatively flexible, making it suitable for the deoxidation treatment of a variety of carbon materials.
[0014] Optionally, in the method for efficiently removing oxygen from carbon materials provided by the present invention, the pressure of the deoxidation reduction reaction is 0.05-5 MPa, and the temperature is 80-150°C.
[0015] Optionally, in the method for efficiently removing oxygen from carbon materials provided by the present invention, the time of the deoxygenation-reduction reaction can be adjusted according to actual conditions. For example, the time of the deoxygenation-reduction reaction recommended by the present invention is 1 to 600 minutes, preferably 5 to 60 minutes.
[0016] Optionally, in the method for efficiently removing oxygen from carbon materials provided by the present invention, in the pressurization and heating steps, the rates of pressurization and heating are not specifically limited and can be adjusted according to factors such as the actual moisture and oxygen content in the carbon material. For example, the pressurization rate can be selected to be 0.1 to 10 KPa / s, and the heating rate can be selected to be 5 to 10°C / min.
[0017] Optionally, in the method for efficiently removing oxygen elements from carbon materials provided by the present invention, in the pressurization and heating step, the carbon material to be deoxidized is placed in an open quartz container, ceramic container or tungsten carbide container, and then the container is placed inside a reactor that can withstand pressure and high temperature (such as a reactor, a tubular furnace, an atmosphere box furnace, a hydrogenation reactor, etc.), in order to prevent the carbon material from being contaminated by the metal wall.
[0018] Optionally, in the method for efficiently removing oxygen from carbon materials provided by the present invention, in order to facilitate the reaction and ensure the deoxidation effect, powdered, granular or flaky carbon materials are usually used, and the particle size of the carbon material is preferably 0.1 μm to 10 mm.
[0019] Optionally, in the method for efficiently removing oxygen from carbon materials provided by the present invention, the oxygen content in the carbon material is 0.05wt% to 10wt%, preferably 0.05wt% to 5wt%, and more preferably 0.05wt% to 2wt%.
[0020] Optionally, in the method for efficiently removing oxygen from carbon materials provided by the present invention, the reducing gas includes an active gas and an inert gas; preferably, the active gas accounts for 0.01% to 100% of the reducing gas by volume, and more preferably 5% to 20%.
[0021] Optionally, in the method for efficiently removing oxygen from carbon materials provided by the present invention, the active gas is selected from at least one of hydrogen, methane, ethane, propane, butane, acetylene, propyne and carbon monoxide;
[0022] The inert gas is selected from at least one of nitrogen, helium, argon and carbon dioxide.
[0023] Optionally, in the method for efficiently removing oxygen from carbon materials provided by the present invention, the carbon material is selected from at least one of activated carbon, carbon fiber, carbon nanotubes, graphene, graphene oxide, graphite oxide, supercapacitor activated carbon, capacitor carbon and artificial graphite.
[0024] Optionally, the method for efficiently removing oxygen from carbon materials provided by the present invention specifically comprises the following steps:
[0025] Pressurization and temperature increase: placing the carbon material into a high-pressure reactor, and filling the high-pressure reactor with reducing gas until the pressure of the high-pressure reactor reaches 0.05-10 MPa, then cutting off the reducing gas, and allowing the carbon material and the reducing gas to undergo a deoxidation reduction reaction at 20-200°C;
[0026] Depressurization: After the deoxidation-reduction reaction is completed, the pressure is released, the reaction by-products are discharged, and the deoxidized carbon material is collected.
[0027] Optionally, in the method for efficiently removing oxygen elements from carbon materials provided by the present invention, a vacuum system can be connected to assist in discharging the reaction by-products (mainly water) and unreacted part of the reducing gas in the high-pressure reactor from the high-pressure reactor. For example, the pressure of the high-pressure reactor can be controlled at 0.1 to 100 KPa (absolute pressure), preferably 10 to 60 KPa, through the vacuum system, and the pressure can be maintained for 1 to 360 minutes before cutting off the connection between the vacuum system and the high-pressure reactor.
[0028] Optionally, in the method for efficiently removing oxygen from carbon materials provided by the present invention, when a vacuum system is used to assist in removing reaction by-products and unreacted reducing gas in the high-pressure reactor, after the pressure reduction step is completed, the interior of the high-pressure reactor is at negative pressure, and the high-pressure reactor can be restored to normal pressure by backfilling reducing gas into the high-pressure reactor to remove the reaction product.
[0029] Compared with the prior art, the present invention has the following advantages:
[0030] 1. The method for efficiently removing oxygen from carbon materials provided by the present invention adopts high-pressure deoxidation treatment, that is, by pressurizing the deoxidation environment, reducing the reaction activation energy, so that the deoxidation reaction can be carried out at a relatively low temperature (low temperature or even room temperature). Since the method reacts under high pressure, the reducing gas can fully contact with the material and diffuse into the interior of the material, thereby increasing the depth of the deoxidation reaction and achieving the deoxidation effect at low temperature, which can avoid high temperature damage to the structure of the carbon material. At the same time, the reducing gas partial pressure can be adjusted according to the structure of the material and different oxygen contents, and the deoxidation reaction efficiency is high, the effect is good, and the cost is low.
[0031] 2. The method provided by the present invention for efficiently removing oxygen from carbon materials adopts the pressurization-decompression technology to fill the reducing gas and separate the reaction by-products. The reducing gas can penetrate deep into the pores of the material to carry out the reduction reaction, with high mass transfer efficiency, which is beneficial to the deoxidation treatment of various porous carbon materials, and has high deoxidation depth, high efficiency and high oxygen removal rate.
[0032] 3. Compared with the traditional high-temperature deoxidation method, the method for efficiently removing oxygen from carbon materials provided by the present invention can save part of the time of the heating-cooling process, improve efficiency, and at the same time save part of the energy consumption caused by heating; conventional reactors can be used, which is easy to scale up and can meet industrial production requirements. BRIEF DESCRIPTION OF THE DRAWINGS
[0033] Figure 1 A schematic diagram of a high-pressure reactor used in the method for efficiently removing oxygen from carbon materials provided by the present invention;
[0034] Description of the drawings: 1. Reducing gas supply source; 2. Pressure controller; 3. Reaction pressure indicator; 4. Vent valve; 5. Vacuum valve; 6. Vacuum generator; 7. Quartz tube; 8. Reactor body; 9. Heating and temperature control system; 10. Reactor cover. DETAILED DESCRIPTION
[0035] The present invention is described in detail below by way of examples. It is necessary to point out that the following examples are only used to further illustrate the present invention and are not to be construed as limiting the scope of protection of the present invention. Those skilled in the art may make some non-essential improvements and adjustments to the present invention based on the above disclosure.
[0036] If no specific experimental steps or conditions are specified in the examples, the conventional experimental steps or conditions described in the literature in this field can be used. If the manufacturer of the reagents or instruments is not specified, they are all commercially available conventional reagents.
[0037] Example 1
[0038] This embodiment provides a method for efficiently removing oxygen from carbon materials by Figure 1 The device shown specifically includes the following steps:
[0039] ① Feeding
[0040] 30 g of powdered porous carbon was placed in a quartz tube 7, and then the quartz tube containing the porous carbon was placed in the reactor body 8. The reactor gland 10 was installed and tightened, and the pressure controller 2, the vent valve 4, and the vacuum valve 5 were kept closed. The specific surface area of the porous carbon was 1650 cm 2 / g, oxygen content of 4.6wt%, particle size of 10-20μm;
[0041] ② Pressurization / temperature increase
[0042] The pressure controller 2 is turned on, and reducing gas is introduced into the reactor through the reducing gas supply source 1 until the pressure reaches 2 MPa (reaction pressure, displayed by the reaction pressure indicator 3, and the pressurization rate is 2 kPa / s). The pressure controller 2 is turned off, and the set temperature of the heating and temperature control system 9 is set to 120° C. (reaction temperature, heating rate 8° C. / min). After reaching this temperature, the deoxidation reduction reaction is carried out at a constant temperature for 20 minutes (reaction time);
[0043] The reducing gas is a mixture of hydrogen (H2) and nitrogen (N2) (the volume ratio of hydrogen to nitrogen is 1:9).
[0044] ③ Blood pressure reduction
[0045] Open the vent valve 4 to reduce the pressure of the reactor to normal pressure, then close the vent valve 4, start the vacuum generator 6, open the vacuum valve 5, control the pressure of the vacuum system to 50 kPa (absolute pressure), maintain the system pressure at a constant temperature for 5 minutes, and close the vacuum valve 5.
[0046] ④Repeat
[0047] Repeat steps ② and ③ 3 times.
[0048] ⑤Discharging
[0049] Open the pressure controller 2 and introduce inert gas (high-purity nitrogen) into the reactor until the pressure reaches normal pressure, then close the pressure controller 2; turn off the heating and temperature control system 9, allow the reactor to cool naturally to room temperature, open the reactor cover 10, and take out the deoxidized porous carbon of the reaction product.
[0050] Example 2
[0051] The method for efficiently removing oxygen from carbon materials provided in this embodiment is similar to that in Example 1, with the only difference being that the repetition of step ④ is omitted in this embodiment, and step ⑤ discharging is performed directly after step ③.
[0052] Example 3:
[0053] The method for efficiently removing oxygen from carbon materials provided in this embodiment is similar to that in Example 1, except that step ④ is omitted and the pressure is not reduced by vacuum. The specific steps of this embodiment are as follows:
[0054] ① Feeding
[0055] 30 g of powdered porous carbon was placed in a quartz tube 7, and then the quartz tube containing the porous carbon was placed in the reactor body 8. The reactor gland 10 was installed and tightened, and the pressure controller 2, the vent valve 4, and the vacuum valve 5 were kept closed. The specific surface area of the porous carbon was 1650 cm 2 / g, oxygen content of 4.6wt%, particle size of 10-20μm;
[0056] ② Pressurization / temperature increase
[0057] Open the pressure controller 2, and introduce reducing gas into the high-pressure reactor through the reducing gas supply source 1 until the pressure reaches 2 MPa (reaction pressure, pressurization rate is 2 kPa / s). Close the pressure controller 2, and set the set temperature of the heating and temperature control system 9 to 120°C (reaction temperature, heating rate is 8°C / min). After reaching this temperature, maintain the temperature for 20 minutes (reaction time) to carry out the deoxidation reduction reaction;
[0058] The reducing gas is a mixture of hydrogen (H2) and nitrogen (N2) (the volume ratio of hydrogen to nitrogen is 1:9).
[0059] ③ Blood pressure reduction
[0060] Open the vent valve 4 to reduce the pressure in the reactor to normal pressure.
[0061] ④Discharging
[0062] The heating and temperature control system 9 is turned off, and after the reactor is cooled naturally to room temperature, the reactor cover 10 is opened to take out the deoxidized porous carbon product.
[0063] Example 4
[0064] The method for efficiently removing oxygen from carbon materials provided in this embodiment adopts Figure 1 The device shown specifically includes the following steps:
[0065] ① Feeding
[0066] Take 50g of powdered activated carbon and put it into the quartz tube 7. Then put the quartz tube filled with activated carbon into the reactor body 8. Install and tighten the reactor cover 10. Keep the pressure controller 2, vent valve 4, and vacuum valve 5 closed. The specific surface area of the activated carbon is 2330cm 2 / g, the oxygen content is 2.81wt%, and the particle size is 30-50μm.
[0067] ② Pressurization / temperature increase
[0068] Open pressure controller 2 and introduce reducing gas, a mixture of hydrogen and nitrogen (hydrogen:nitrogen volume ratio of 1:9), into the reactor via reducing gas supply source 1 until the pressure reaches 8 MPa (reaction pressure, pressurization rate of 5 kPa / s). Then close pressure controller 2. Set the set point temperature of heating and temperature control system 9 to 60°C (reaction temperature, heating rate of 2°C / min). After reaching this temperature, maintain the temperature for 50 minutes (reaction time) to carry out the deoxidation reduction reaction.
[0069] ③ Blood pressure reduction
[0070] Open the vent valve 4 to reduce the pressure of the reactor to normal pressure, then close the vent valve 4, start the vacuum generator 6, open the vacuum valve 5, control the pressure of the vacuum system to 40KPa (reduced pressure), maintain the system pressure at a constant temperature for 10 minutes (reduced pressure time), and close the vacuum valve 5.
[0071] ④Repeat
[0072] Repeat steps ② and ③ 4 times.
[0073] ⑤Discharging
[0074] Open the pressure controller 2 and introduce inert gas (high-purity nitrogen) into the reactor until the pressure reaches normal pressure, then close the pressure controller 2; turn off the heating and temperature control system 9, allow the reactor to cool naturally, open the reactor gland 10, and take out the deoxygenated activated carbon of the reaction product.
[0075] Example 5
[0076] This embodiment provides a method for efficiently removing oxygen from carbon materials by Figure 1 The device shown specifically includes the following steps:
[0077] ① Feeding
[0078] 5 g of powdered graphene was placed in a quartz tube 7, and then the quartz tube containing graphene was placed in the reactor body 8. The reactor gland 10 was installed and tightened, and the pressure controller 2, the vent valve 4, and the vacuum valve 5 were kept closed. The specific surface area of the graphene was 1215 cm 2 / g, and the oxygen content is 14.05wt%.
[0079] ② Pressurization / temperature increase
[0080] Open the pressure controller 2, and introduce reducing gas into the reactor through the reducing gas supply source 1 until the pressure reaches 0.8 MPa (reaction pressure, pressurization rate is 0.2 KPa / s). Close the pressure controller 2, set the set temperature of the heating and temperature control system 9 to 150°C (reaction temperature, heating rate is 6°C / min), and after reaching this temperature, maintain the temperature for 10 minutes (reaction time) to carry out the deoxidation reduction reaction;
[0081] The reducing gas is a mixture of hydrogen (H2), methane (CH4) and nitrogen (N2) (the volume ratio of hydrogen, methane and nitrogen is 1:1:8).
[0082] ③ Blood pressure reduction
[0083] Open the vent valve 4 to reduce the pressure of the reactor to normal pressure, then close the vent valve 4, start the vacuum generator 6, open the vacuum valve 5, control the pressure of the vacuum system to 40KPa (reduced pressure), maintain the system pressure at a constant temperature for 15 minutes, and close the vacuum valve 5.
[0084] ④Repeat
[0085] Repeat steps ② and ③ 3 times.
[0086] ⑤Discharging
[0087] Open the pressure control regulator 2 and introduce inert gas (high-purity nitrogen) into the reactor until the pressure reaches normal pressure, then close the pressure controller 2; turn off the heating and temperature control system 9, allow the reactor to cool naturally to room temperature, open the reactor cover 10, and take out the deoxidized graphene reaction product.
[0088] Comparative Example 1
[0089] The method for efficiently removing oxygen from carbon materials provided in this comparative example is similar to that in Example 3. Figure 1 The device shown specifically includes the following steps:
[0090] ① Feeding
[0091] 30 g of powdered porous carbon was placed in a quartz tube 7, and then the quartz tube containing the porous carbon was placed in the reactor body 8. The reactor gland 10 was installed and tightened, and the pressure controller 2, the vent valve 4, and the vacuum valve 5 were kept closed. The specific surface area of the porous carbon was 1650 cm 2 / g, oxygen content of 4.6wt%, particle size of 10-20μm;
[0092] ②Heating
[0093] Open the vent valve 4, open the pressure controller 2, and continuously introduce reducing gas into the reactor through the reducing gas supply source 1 to control the reaction to proceed under normal pressure. Start the heating and temperature control system 9 and set the set temperature to 120°C (reaction temperature). After reaching this temperature, keep the temperature constant for 20 minutes (reaction time) to carry out the deoxygenation reaction;
[0094] The reducing gas is a mixture of hydrogen (H2) and nitrogen (N2) (the volume ratio of hydrogen to nitrogen is 1:9).
[0095] ③Discharging
[0096] Turn off the pressure control regulator 2, turn off the heating and temperature control system 9, wait for the reactor to cool naturally to room temperature, open the reactor cover 10, and take out the deoxidized porous carbon product.
[0097] Comparative Example 2
[0098] The method for efficiently removing oxygen from carbon materials provided in this comparative example is similar to that in comparative example 1, with the only difference being that the deoxidation reaction time in the heating step ② in this comparative example is 90 minutes.
[0099] Comparative Example 3
[0100] The method for efficiently removing oxygen from carbon materials provided in this comparative example is similar to that in comparative example 1, with the only difference being that the deoxidation reaction temperature in the heating step ② in this comparative example is 800°C.
[0101] Table 1 Raw materials, treatment processes and products in Examples and Comparative Examples
[0102]
[0103] Note: The specific surface area of the material is tested using a nitrogen adsorption instrument, and the oxygen content is tested using a high-temperature element analyzer.
[0104] It can be seen from the data in the above table that in Example 1, after repeated pressurization and depressurization, vacuum-assisted decompression and other operations, the final oxygen removal rate of the porous carbon can reach more than 97%; in Example 2, no repeated treatment process was performed, and in Example 3, no vacuum-assisted decompression and repeated process were used, but the oxygen content of the product can still reach a low level, and the specific surface area of the carbon material before and after deoxygenation treatment does not change much, indicating that the structure of the material is not affected, and the oxygen content in the carbon material can be further reduced to an extremely low level through vacuum-assisted decompression and repeated pressurization and decompression.
[0105] Examples 1-3, Example 4, and Example 5 illustrate that the deoxidation method provided by the present invention can achieve good deoxidation effects in carbon materials such as porous carbon, activated carbon, and graphene, indicating that the deoxidation method provided by the present invention has excellent universality for carbon materials of different types and with different oxygen contents. Comparison of Example 1 with Example 3 shows that, since Comparative Example 1 does not use a pressurization process, the oxygen content of the porous carbon material after treatment is much higher than that of Example 3; in Comparative Examples 2 and 3, the reaction time or reaction temperature is greatly increased, but the oxygen content is still significantly higher than that of Example 3, indicating that the deoxidation effect of the traditional high-temperature deoxidation method is poor, and the specific surface area of the material in Comparative Example 3 decreases more than that of Examples 1 to 3, indicating that the reaction at high temperature has damaged the structure of the material.
[0106] In summary, from the comparison of the data of Examples 1-5 and Comparative Examples 1-3, it can be seen that the deoxidation method provided by the present invention can treat various carbon materials and achieve good deoxidation effects without destroying the structure of the carbon materials.
[0107] Of course, the present invention may have many other embodiments. Without departing from the spirit and essence of the present invention, those skilled in the art may make various corresponding changes and modifications based on the present invention, but these corresponding changes and modifications should all fall within the scope of protection of the claims of the present invention.
Claims
1. A method for efficiently removing oxygen from carbon materials, characterized in that: The steps include: Pressurization and temperature increase: placing the carbon material into a high-pressure reactor, and filling the high-pressure reactor with reducing gas until the gauge pressure of the high-pressure reactor reaches 0.05-10 MPa, then cutting off the reducing gas, and allowing the carbon material and the reducing gas to undergo a deoxidation reduction reaction at 80-150°C for 1-600 min; Depressurization: performing a temperature and pressure reduction treatment on the carbon material after the deoxidation reduction reaction is completed; After the steps of pressurizing, heating and reducing pressure are repeated 0 to 10 times, the carbon material after the oxygen element is removed is obtained.
2. The method for efficiently removing oxygen from carbon materials according to claim 1, wherein: The gauge pressure of the deoxidation reduction reaction is 0.05~5MPa.
3. The method for efficiently removing oxygen from carbon materials according to claim 1, wherein: The deoxidation reduction reaction time is 5 to 60 min.
4. The method for efficiently removing oxygen from carbon materials according to claim 1, wherein: In the pressurization and temperature increase step, the pressurization rate is 0.1-10 KPa / s, and the temperature increase rate is 5-10°C / min.
5. The method for efficiently removing oxygen from carbon materials according to claim 1, wherein: The carbon material is in the form of powder, flake or granule.
6. The method for efficiently removing oxygen from carbon materials according to claim 1, wherein: The oxygen content in the carbon material is 0.05 wt % to 10 wt %.
7. The method for efficiently removing oxygen from carbon materials according to claim 1, wherein: The reducing gas includes active gas and inert gas.
8. The method for efficiently removing oxygen from carbon materials according to claim 7, wherein: In terms of volume ratio, the active gas accounts for 0.01% to 100% of the reducing gas.
9. The method for efficiently removing oxygen from carbon materials according to claim 7, wherein: The active gas is selected from at least one of hydrogen, methane, ethane, propane, butane, acetylene, propyne and carbon monoxide; The inert gas is selected from at least one of nitrogen, helium, argon and carbon dioxide.
10. The method for efficiently removing oxygen from carbon materials according to claim 1, wherein: The carbon material is selected from at least one of activated carbon, carbon fiber, carbon nanotube, graphene, graphene oxide, graphite oxide, supercapacitor activated carbon, capacitor carbon and artificial graphite.
11. The method for efficiently removing oxygen from carbon materials according to claim 5, wherein: The particle size of the carbon material is 0.1 μm to 10 mm.
12. The method for efficiently removing oxygen from carbon materials according to claim 8, wherein: In terms of volume ratio, the active gas accounts for 5% to 20% of the reducing gas.