Porous carbon material preparation device
By designing a porous carbon material preparation device with a closed structure and an inert gas environment, the temperature control difficulty and oxidation risks caused by the exposure of the top of the template are solved, and efficient and stable preparation of porous carbon materials is achieved.
Patent Information
- Application Number
- CN202422570912.4
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- Filing Date
- 2024-10-23
- Publication Date
- 2025-09-05
- Estimated Expiration
- 2034-10-23
AI Technical Summary
In the existing ice template freezing device, the direct exposure of the top of the template to the air makes it difficult to control the temperature and the risk of oxidation of the precursor liquid.
Design a porous carbon material preparation device, including liquid nitrogen refrigeration containers, molds and elastic containers, adopt a closed structure and an inert gas environment, preventing the precursor liquid from contacting with oxygen, providing rapid cooling through liquid nitrogen refrigeration containers, and providing a stable frame to ensure shape and size accuracy.
It realizes efficient preparation of porous carbon materials, ensures accurate temperature control, prevents oxidation reactions, improves the consistency and repeatability of materials, and reduces operational difficulty and maintenance costs.
Smart Images

Figure CN223307143U_ABST
Abstract
Description
Technical Field
[0001] The utility model relates to the technical field of material preparation, in particular to a device for preparing porous carbon materials. Background Art
[0002] Porous materials are materials with a network structure consisting of interconnected or closed pores. These materials primarily consist of a continuous solid phase, which forms the material's basic structure, and a fluid phase, which forms the pores. Compared to continuous, non-porous materials, these materials generally offer lower relative density, higher specific strength, larger specific surface area, and better sound absorption, thermal insulation, and permeability. Consequently, they are widely used in applications such as adsorption, separation, support, support, noise reduction, and thermal insulation.
[0003] Porous carbon materials, due to their unique structure and excellent properties, are gradually becoming an important part of modern materials science and engineering. Factors affecting the structure of porous carbon materials include the chemical composition and physical properties of the raw materials, the preparation process, the carbonization temperature and time, and the post-treatment method. Different raw materials will lead to large differences in the porosity and specific surface area of carbon materials; the preparation method and operation process directly affect the morphology, structure and size of the pores; the carbonization and post-treatment processes have a significant impact on the crystal structure of carbon materials and the stability of their pores. Although porous carbon materials have shown excellent performance in various applications, they still have disadvantages such as high cost, process complexity, low yield and potential environmental hazards in the precise preparation of porous carbon materials with specific structures and morphologies. Therefore, optimizing the preparation process and selecting appropriate preparation equipment to promote the precise control of porous carbon materials and their development towards a more efficient and sustainable direction have become the focus of current research.
[0004] Ice templating, a novel technique for preparing three-dimensional porous materials, relies on template structures formed during ice crystal growth to create porous materials with controllable morphology and structure. It is gaining attention due to its ease of operation, simple material preparation, ease of scale-up, and environmental friendliness. The basic principle is that as ice crystals grow in a solution, they arrange solute molecules in an orderly manner at the interface between the ice crystal and the solution, forming a template with a specific shape and size. As the ice crystals melt, these template structures are preserved, enabling the preparation of porous materials.
[0005] In a patent entitled "An automated rapid freezing device based on the ice template method" and with publication number CN212619533U, a freezing device with a liquid nitrogen freezing container and a heating ring for regulating the temperature field is disclosed. The liquid nitrogen freezing container can provide a low temperature of more than one hundred degrees Celsius below zero. As a cooling end, it can expand the adjustable temperature gradient between it and the heating ring as the heating end. The patent can form a temperature gradient from low to high, combined with a bottom-up temperature gradient formed by the liquid nitrogen freezing container. The two temperature gradients jointly limit the random orientation growth of ice crystals in a two-dimensional plane. However, the technical solution disclosed in the patent still has the following problems: the top is directly exposed to the air, and there is difficulty in temperature control due to heat exchange with the outside world due to the lack of insulation material. There is also a risk of oxidation of the precursor liquid, which is not a good choice for reactive precursor liquids. Utility Model Content
[0006] The present invention aims to solve at least one of the technical problems existing in the prior art. To this end, the present invention provides a porous carbon material preparation device, which aims to solve the problem that the top of the template in the related art freezing device based on the ice template method is directly exposed to the air, making it difficult to control the temperature of the precursor solution and posing a risk of oxidation to the precursor solution.
[0007] The utility model provides a porous carbon material preparation device, comprising:
[0008] A liquid nitrogen freezing container, wherein a freezing port is provided on the top of the liquid nitrogen freezing container;
[0009] A mold, wherein the mold is arranged on the top of the liquid nitrogen freezing container, the bottom of the mold covers the freezing port, and the top of the mold is provided with an air outlet and an openable and closable air inlet;
[0010] An elastic container is used for being detachably connected to the air outlet.
[0011] According to the porous carbon material preparation device provided by the present invention, the liquid nitrogen freezing container includes an inner shell, an outer shell and an insulation layer, the interior of the inner shell forms a first cavity for accommodating liquid nitrogen, the freezing port is used to connect the inner and outer sides of the first cavity, the outer shell is coated on the outside of the inner shell, and a closed second cavity is formed between the inner shell and the outer shell, and the insulation layer is filled in the second cavity.
[0012] According to the porous carbon material preparation device provided by the present invention, the top surface of the liquid nitrogen freezing container is further provided with a rib, which surrounds the edge of the liquid nitrogen freezing container and the top of the rib is higher than the top surface of the liquid nitrogen freezing container.
[0013] According to the porous carbon material preparation device provided by the present invention, the mold includes:
[0014] an insulating shell having an open top and a bottom;
[0015] a heat-conducting base, the heat-conducting base being used to be placed on top of the liquid nitrogen freezing container, with the bottom of the heat-conducting base completely covering the freezing port, and the heat-insulating shell being arranged on top of the heat-conducting base and in sealing contact with the heat-conducting base;
[0016] The heat-insulating sealing cover is used to detachably seal the top of the heat-insulating shell, and the air inlet and the air outlet are arranged on the heat-insulating sealing cover.
[0017] According to the porous carbon material preparation device provided by the present invention, a groove is provided on the top of the heat-conducting base, and the bottom of the heat-insulating shell is used to be inserted into the groove. When the bottom of the heat-insulating shell is inserted into the groove, the outer side surface of the heat-insulating shell is sealed to the inner side surface of the groove, and the bottom surface of the heat-insulating shell is sealed to the bottom surface of the groove.
[0018] According to the porous carbon material preparation device provided by the present invention, a detachable air inlet plug is provided at the air inlet, and when the air inlet plug is inserted into the air inlet, the air inlet is closed.
[0019] According to the porous carbon material preparation device provided by the utility model, an outlet plug is provided at the outlet, a gas channel is provided on the outlet plug, and the elastic container is used to be detachably connected to the outlet plug and communicate with the interior of the thermal insulation shell through the gas channel.
[0020] According to the porous carbon material preparation device provided by the present invention, the heat-insulating shell, the heat-insulating sealing cover, the air inlet plug and the air outlet plug are all made of polytetrafluoroethylene.
[0021] According to the porous carbon material preparation device provided by the present invention, the material of the heat-conducting base is copper.
[0022] According to the porous carbon material preparation device provided by the present invention, the elastic container is a balloon.
[0023] The utility model has the following advantages due to the adoption of the above technical solution:
[0024] The porous carbon material preparation device provided by the utility model includes a liquid nitrogen freezing container, a mold and an elastic container. The top of the liquid nitrogen freezing container is provided with a freezing port, the mold is arranged on the top of the liquid nitrogen freezing container, and the bottom of the mold covers the freezing port. The liquid nitrogen in the liquid nitrogen freezing container provides coldness to the precursor liquid in the mold through the freezing port, so that the precursor liquid in the mold is quickly cooled. An air outlet and a closable air inlet are provided at the top of the mold, and the elastic container is detachably arranged at the air outlet. When preparing the porous carbon material, the configured precursor liquid is first poured into the mold, and then an inert gas is injected into the mold through the air inlet. After the air in the mold is evacuated, the elastic container is connected to the air outlet. When the elastic container expands, the supply of inert gas is stopped, and the air inlet is then closed. Liquid nitrogen is then added to the liquid nitrogen freezing container, and the mold is placed at the freezing port, waiting for freezing to complete. The frozen porous carbon material is then demoulded, and a longitudinal channel is left after the ice crystals sublime. Finally, the porous carbon material is carbonized to obtain the final porous carbon material. In the porous carbon material preparation device provided by the present invention, a liquid nitrogen freezing container is used for rapid cooling to ensure that a uniform and delicate ice template is formed during the preparation process. The mold provides a stable frame for supporting and fixing the required raw materials, while ensuring the accuracy of the shape and size of the template. Moreover, the mold can ensure the airtightness of the internal environment throughout the preparation process, preventing external factors from affecting the process of preparing porous carbon materials from the ice template, thereby ensuring the high consistency and repeatability of the porous carbon material. The porous carbon material preparation device can provide a closed inert gas environment, effectively preventing the precursor liquid from contacting with oxygen during the freezing process, thereby avoiding the potential impact of the oxidation reaction on the precursor liquid. The porous carbon material preparation device is easy to move and place in different working environments. This design not only improves the convenience of operation, but also reduces maintenance costs, allowing the device to maximize its effectiveness in various application scenarios. BRIEF DESCRIPTION OF THE DRAWINGS
[0025] In order to more clearly illustrate the technical solutions of the present invention or the prior art, the following briefly introduces the drawings required for use in the embodiments or the description of the prior art. Obviously, the drawings described below are some embodiments of the present invention. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying any creative work.
[0026] Figure 1 This is a schematic structural diagram of a porous carbon material preparation device provided by one embodiment of the present invention;
[0027] Figure 2 This is an exploded view of a porous carbon material preparation device provided by one embodiment of the present utility model;
[0028] Figure 3This is a cross-sectional view of a porous carbon material preparation device provided by one embodiment of the present invention;
[0029] Figure 4 This is a cross-sectional view of a liquid nitrogen freezing container provided by one embodiment of the present utility model;
[0030] Figure 5 This is a schematic diagram of the microstructure of the porous carbon material provided by an embodiment of the present invention. Figure 1 ;
[0031] Figure 6 This is a schematic diagram of the microstructure of the porous carbon material provided by an embodiment of the present invention. Figure 2 ;
[0032] Figure 7 This is a schematic diagram of the microstructure of the porous carbon material provided by an embodiment of the present invention. Figure 3 ;
[0033] Figure 8 This is the N2 adsorption-desorption isotherm of the porous carbon material catalyst provided in one embodiment of the present invention.
[0034] Reference numerals:
[0035] 100: Liquid nitrogen freezing container; 110: Inner shell; 120: Outer shell; 130: Top plate; 131: Freezing port; 132: Side dam; 140: Insulation layer; 210: Insulated shell; 220: Heat-conducting base; 221: Groove; 230: Insulated sealing cover; 231: Air inlet; 232: Air outlet; 300: Elastic container; 410: Air outlet plug; 411: Gas channel; 420: Air inlet plug. DETAILED DESCRIPTION
[0036] To make the purpose, technical solutions, and advantages of the present invention more clear, the following will be combined with the accompanying drawings to clearly and completely describe the technical solutions of the present invention. Obviously, the embodiments described are only some of the embodiments of the present invention, not all of them. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making creative efforts are within the scope of protection of the present invention.
[0037] In the description of the present invention, it should be understood that the terms "center", "longitudinal", "lateral", "length", "width", "thickness", "up", "down", "front", "back", "left", "right", "vertical", "horizontal", "top", "bottom", "inside", "outside", "clockwise", "counterclockwise", "axial", "radial", "circumferential" and the like to indicate orientations or positional relationships based on the orientations or positional relationships shown in the accompanying drawings, and are only for the convenience of describing the present invention and simplifying the description, and do not indicate or imply that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation, and therefore should not be understood as a limitation to the present invention.
[0038] Furthermore, the terms "first" and "second" are used for descriptive purposes only and should not be construed as indicating or implying relative importance or implicitly specifying the number of the technical features being referred to. Thus, a feature specified as "first" or "second" may explicitly or implicitly include one or more of such features. In the description of this utility model, "plurality" means more than two, unless otherwise specifically defined.
[0039] In this utility model, unless otherwise specified or limited, the terms "installed," "connected," "connect," "fixed," etc. should be understood in a broad sense. For example, they can refer to fixed connection, detachable connection, or integration; mechanical connection, electrical connection; direct connection, indirect connection through an intermediate medium; internal communication between two components, or interaction between two components. Those skilled in the art will understand the specific meanings of the above terms in this utility model based on specific circumstances.
[0040] In the present invention, unless otherwise expressly specified or limited, when a first feature is "above" or "below" a second feature, it may mean that the first and second features are in direct contact, or the first and second features are in indirect contact through an intermediary. Furthermore, when a first feature is "above," "above," or "above" a second feature, it may mean that the first feature is directly above or diagonally above the second feature, or simply means that the first feature is at a higher level than the second feature. When a first feature is "below," "below," or "below" a second feature, it may mean that the first feature is directly below or diagonally below the second feature, or simply means that the first feature is at a lower level than the second feature.
[0041] In the description of this specification, the description with reference to the terms "one embodiment", "some embodiments", "example", "specific example", or "some examples" means that the specific features, structures, materials or characteristics described in conjunction with the embodiment or example are included in at least one embodiment or example of the present invention. In this specification, the schematic representations of the above terms do not necessarily refer to the same embodiment or example. Moreover, the specific features, structures, materials or characteristics described can be combined in any one or more embodiments or examples in a suitable manner. In addition, those skilled in the art can combine and combine different embodiments or examples described in this specification and features of different embodiments or examples without contradiction.
[0042] The utility model provides a porous carbon material preparation device, comprising a liquid nitrogen freezing container, a mold and an elastic container. A freezing port is provided on the top of the liquid nitrogen freezing container, the mold is provided on the top of the liquid nitrogen freezing container and covers the freezing port, and an air outlet and an openable and closable air inlet are provided on the top of the mold. The elastic container is used to be detachably connected to the air outlet. The liquid nitrogen in the liquid nitrogen freezing container provides cooling to the precursor liquid in the mold through the freezing port, causing it to cool down quickly. The mold provides a stable frame for supporting and fixing the required raw materials while ensuring the accuracy of the shape and size of the template. The air inlet at the top of the mold can be used to fill the mold with inert gas before freezing, and the air outlet is used to exhaust air. When the air is exhausted, the elastic container is connected to the air outlet. When the elastic container expands, the supply of inert gas is stopped and the air inlet is closed. The porous carbon material preparation device provided by the utility model provides a closed inert gas environment for the precursor liquid, so that the internal precursor liquid is protected from the influence of the external environment, making it easier to control the temperature, and the inert gas environment can prevent the precursor liquid from oxidizing.
[0043] The following combination Figures 1 to 8 The present invention describes a porous carbon material preparation device.
[0044] An embodiment of the present invention provides a porous carbon material preparation device, which includes a liquid nitrogen freezing container 100 , a mold, and an elastic container 300 .
[0045] The liquid nitrogen freezing container 100 is used to contain liquid nitrogen. A freezing port 131 is provided on the top thereof. The freezing port 131 is connected to the interior of the liquid nitrogen freezing container 100. The liquid nitrogen freezing container 100 can exchange heat with an external device through the freezing port 131 to provide cooling for the external device.
[0046] The mold is used to hold the precursor liquid. The mold is set on the top of the liquid nitrogen freezing container 100, and the bottom of the mold covers the freezing port 131 of the liquid nitrogen freezing container 100. The coldness of the liquid nitrogen freezing container 100 is transferred to the precursor liquid in the mold through heat conduction, so that the precursor liquid is quickly cooled.
[0047] An air outlet 232 and an openable and closable air inlet 231 are provided on the top of the mold. The air inlet 231 can be used to fill the mold with inert gas and discharge the air in the mold through the air outlet 232.
[0048] The elastic container 300 is detachably connected to the air outlet 232 . When the air in the mold is exhausted and the mold is filled with inert gas, the elastic container 300 can be connected to the air outlet 232 . After the elastic container 300 expands, the supply of inert gas is stopped.
[0049] The preparation process of porous materials is as follows:
[0050] Prepare a precursor solution. For example, the aqueous phase can be a 5% ER-10 solution prepared by mixing ER-10 emulsifier with water. Weigh 100 mg of carbon black and 50 mg of graphene oxide and dissolve them in the aqueous phase. After ultrasonic treatment for 5 minutes, add 200 mg of sodium carboxymethyl cellulose and place in a magnetic stirrer. Mix and stir thoroughly to obtain a stably dispersed precursor solution.
[0051] Pour the precursor liquid into the mold, then open the air inlet 231 and introduce inert gas into the mold. After the air in the mold is emptied, install the elastic container 300 at the air outlet 232 and continue to introduce inert gas. When the elastic container 300 expands, stop supplying inert gas and close the air inlet 231.
[0052] Liquid nitrogen is added into the liquid nitrogen freezing container 100, and the mold is placed at the freezing port 131 on the top of the liquid nitrogen freezing container 100, and the freezing is waited for to be completed.
[0053] The frozen porous carbon material is demoulded and placed in a freeze dryer for 24 hours to allow the ice crystals to sublime directly, leaving behind longitudinal channels.
[0054] Finally, the porous carbon material is carbonized, the temperature is raised to 600°C at a heating rate of 5°C / min, kept at this temperature for 6 hours, and cooled in the furnace to finally obtain a porous carbon material with a directional pore structure.
[0055] The porous carbon material preparation device provided by the embodiment of the present utility model is intended to improve the preparation efficiency and quality of porous carbon materials. The device mainly includes a liquid nitrogen freezing container 100, a mold and an elastic container 300. The liquid nitrogen freezing container 100 is used for rapid cooling to ensure that a uniform and delicate ice template is formed during the preparation process. The mold provides a stable frame for supporting and fixing the required raw materials while ensuring the accuracy of the shape and size of the template. The mold also provides a closed environment to prevent external factors from affecting the process of preparing porous carbon materials from the ice template, thereby ensuring the high consistency and repeatability of the porous carbon material. The device can also be introduced with inert gas to form a closed inert gas environment inside the mold, which can effectively prevent the precursor liquid from contacting with oxygen during the freezing process, thereby avoiding the potential impact of the oxidation reaction on the precursor liquid. The device is easy to move and place in different working environments. This design not only improves the convenience of operation, but also reduces maintenance costs, so that the device can maximize its effectiveness in various application scenarios.
[0056] In some embodiments of the present invention, a liquid nitrogen freezing container 100 includes an inner shell 110, an outer shell 120, and an insulation layer 140. The interior of the inner shell 110 forms a first cavity for accommodating liquid nitrogen. A freezing port 131 is disposed at the top of the inner shell 110 and connects the inside and outside of the first cavity. The outer shell 120 covers the exterior of the inner shell 110, forming a closed second cavity between the inner shell 110 and the outer shell 120. The insulation layer 140 fills the second cavity.
[0057] Specifically, both the inner shell 110 and the outer shell 120 can be cylindrical structures with a hollow interior and an open top. The outer diameter of the inner shell 110 is smaller than the inner diameter of the outer shell 120, and the height of the inner shell 110 is smaller than the height of the outer shell 120. During installation, the inner shell 110 and the outer shell 120 are arranged coaxially, and the tops of the inner shell 110 and the outer shell 120 are flush. A top plate 130 is provided on the tops of the inner shell 110 and the outer shell 120. The top plate 130 is an annular plate with an inner diameter less than or equal to the inner diameter of the inner shell 110, and an outer diameter that can be greater than the outer diameter of the outer shell 120. When connected, the top plate 130 is coaxial with the inner shell 110, and the tops of the inner shell 110 and the outer shell 120 are both connected to the bottom surface of the top plate 130. The area between the top plate 130 and the inner shell 110 forms a first cavity, and the hole in the center of the top plate 130 forms a freezing port 131 connecting the inside and outside of the first cavity. The space between the inner shell 110 and the outer shell 120 forms a second cavity, which is filled with an insulation layer 140.
[0058] In some embodiments of the present invention, a rib 132 is further provided on the top surface of the liquid nitrogen freezing container 100 . The rib 132 surrounds the edge of the liquid nitrogen freezing container 100 , and the top of the rib 132 is higher than the top surface of the liquid nitrogen freezing container 100 .
[0059] Specifically, the rib 132 can be a cylinder with a hollow interior and open top and bottom. The outer diameter of the rib 132 can be equal to the outer diameter of the top plate 130 . The rib 132 is coaxially arranged with the top plate 130 and welded to the top edge of the top plate 130 .
[0060] The retaining edge 132 can prevent the liquid nitrogen spilled outside from dripping when the liquid nitrogen is added through the freezing port 131 .
[0061] In some embodiments of the present invention, the mold includes a heat-insulating shell 210 , a heat-conducting base 220 and a heat-insulating sealing cover 230 .
[0062] The heat-insulating shell 210 may be a rectangular parallelepiped structure with a hollow interior and open top and bottom. The heat-insulating shell 210 may be made of polytetrafluoroethylene.
[0063] The heat-conducting base 220 is used to be placed on the top of the liquid nitrogen freezing container 100 and to completely cover the freezing port 131. The heat-insulating shell 210 is disposed on the top of the heat-conducting base 220 and is in sealed contact with the heat-conducting base 220.
[0064] Since the heat-conducting base 220 is used to seal the freezing port 131 and the bottom opening of the heat-insulating shell 210 and to conduct heat, the heat-conducting base 220 can be of any shape as long as it can seal the freezing port 131 and the bottom opening of the heat-insulating shell 210. Since the heat-conducting base 220 needs to conduct heat to transfer the cold energy from the liquid nitrogen freezing container 100 to the precursor liquid in the mold, copper with good thermal conductivity can be used for the heat-conducting base 220.
[0065] The heat-insulating sealing cover 230 is used to detachably seal the top of the heat-insulating housing 210, and the air inlet 231 and the air outlet 232 are provided on the heat-insulating sealing cover 230. The heat-insulating sealing cover 230 is used to seal the top of the heat-insulating housing 210 and inject inert gas into the heat-insulating housing 210 through the air inlet 231, thereby expelling the internal air through the air outlet 232.
[0066] In some embodiments of the present invention, a groove 221 is provided on the top of the heat-conducting base 220, and the bottom of the heat-insulating shell 210 is configured to be inserted into the groove 221. When the bottom of the heat-insulating shell 210 is inserted into the groove 221, the outer side surface of the heat-insulating shell 210 is sealed against the inner side surface of the groove 221, and the bottom surface of the heat-insulating shell 210 is sealed against the bottom surface of the groove 221.
[0067] Specifically, a rectangular groove 221 is provided at the bottom of the heat-conducting base 220. The cross-sectional shape and dimensions of the groove 221 are identical to those of the heat-insulating housing 210. Thus, the bottom of the heat-insulating housing 210 can be inserted downwardly into the groove 221, so that the outer side of the heat-insulating housing 210 seals against the inner side of the groove 221, and the bottom of the heat-insulating housing 210 seals against the bottom of the groove 221, thereby sealing the heat-conducting base 220 against the bottom opening of the heat-insulating housing 210.
[0068] In some embodiments of the present invention, a removable air inlet plug 420 may be provided at the air inlet 231. The air inlet plug 420 may be plugged into the air inlet 231 and may be made of polytetrafluoroethylene. When inert gas needs to be supplied to the mold, the air inlet plug 420 is removed and connected to a pipeline from the inert gas source. When the inert gas supply is stopped and the mold needs to be sealed, the air inlet plug 420 is inserted into the air inlet 231 to seal the mold.
[0069] In some embodiments of the present invention, an air outlet plug 410 can be provided at the air outlet 232, and a gas channel 411 is provided on the air outlet plug 410. The elastic container 300 can be a balloon, and the air inlet and outlet of the balloon can be detachably connected to the air outlet plug 410. After connection, the gas channel 411 of the air outlet plug 410 is connected to the interior of the balloon.
[0070] Specifically, the outlet plug 410 is used to connect the balloon to the outlet 232. The tip of the outlet plug 410 is inserted into the outlet 232, and the tail is connected to the gas inlet and outlet. After the air in the mold is exhausted, the outlet plug 410 with the balloon attached can be inserted into the outlet 232. The inert gas supply continues. After the balloon is inflated, the inert gas supply is stopped, and the inlet plug 420 is inserted into the inlet 231.
[0071] The balloon can maintain positive pressure at the air inlet 231 when the inert gas pipeline is removed and the air inlet plug 420 is inserted, thereby preventing external air from entering the mold.
[0072] like Figure 5 As shown, Figure 5 The microstructure of the porous carbon material, obtained using a scanning electron microscope, is shown. Due to the vertical temperature gradient, the solvent water grows in a directional manner, forming flaky ice crystals. Simultaneously, solutes such as carbon black and graphene oxide in the precursor solution are repelled, approached, and compressed by the ice crystals, forming a layered structure. The microstructure is observed to be a layered structure with mesopores, with gaps of 20-30μm.
[0073] By varying the concentration of ER-10, polyaniline layered structures with varying pore sizes can be obtained, providing a new approach for manipulating material properties. As the concentration of ER-10 increases, the degree of polymerization and interactions of polyaniline change, affecting the resulting pore size. Higher concentrations of ER-10 generally result in a more compact structure and smaller pores, while lower concentrations favor larger pores.
[0074] like Figure 6 and Figure 7 As shown, Figure 6 Scanning electron microscope image of porous carbon material with ER-10 content of 2%. Figure 7 Scanning electron microscope image of porous carbon material with ER-10 content of 8%.
[0075] The specific surface area size of the porous carbon material and the pore structure on the material wall were further analyzed through BET specific surface area test data. Figure 8 This is the N2 adsorption-desorption isotherm of the porous carbon material catalyst. The figure shows that the pore size on the porous carbon material wall exhibits a Type IV isotherm, indicating the presence of mesopores with a size of 2-50nm on the porous carbon material wall. Furthermore, the sample exhibits an H4-type hysteresis loop, which indirectly confirms the presence of a mesoporous structure on the material surface. Furthermore, according to the pore size distribution curve in the figure, it can be seen that the pore size is mainly distributed around 2-4nm and 30nm, with a large number of micropores and mesoporous structures, which helps to improve the hydrophilic properties of the porous carbon material.
[0076] The porous carbon material preparation device provided by the present invention improves the freezing efficiency by injecting liquid nitrogen. Liquid nitrogen has an extremely low temperature (about -196°C) and can achieve a rapid and uniform freezing process in a short time. By adopting liquid nitrogen injection technology, the device can significantly improve the freezing efficiency and ensure that the carbon material in the ice template forms a small and uniform pore structure during the freezing process. The porous material prepared by this method has a high specific surface area and a regular pore structure. This regular pore structure not only helps to improve the metal loading capacity, but also promotes synergy between metals, making the catalyst more efficient. In addition, due to the integrated molding of the porous carbon material, the catalyst has higher mechanical strength and toughness, thereby ensuring the stability of the catalytic effect. Finally, the preparation process of this device is simple, without tedious preparation steps, and is therefore more efficient.
[0077] The porous carbon material preparation device provided by this utility model effectively isolates the precursor liquid from oxygen during the freezing process. This device uses a sealed structure and gas isolation technology to ensure that the precursor liquid does not come into contact with oxygen during the freezing process, avoiding the potential impact of oxidation reactions on the precursor liquid quality.
[0078] In addition, the porous carbon material preparation device provided by the present invention also has the advantages of portability and simple assembly. In terms of design, the structure of the device is lightweight and modular, and the molds are composed of small polytetrafluoroethylene modules, making it easy to move and place in different working environments. The modular design not only improves the convenience of operation, but also reduces maintenance costs. The device has a compact structure and adopts a modular design, which is easy to disassemble and move. This design allows the device to be quickly installed and adjusted in different working environments, improving the flexibility and efficiency of operation.
[0079] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present application, rather than to limit them. Although the present application has been described in detail with reference to the aforementioned embodiments, those skilled in the art should understand that they can still modify the technical solutions described in the aforementioned embodiments, or make equivalent replacements for some or all of the technical features therein. These modifications or replacements do not deviate the essence of the corresponding technical solutions from the scope of the technical solutions of the embodiments of the present application, and they should all be included in the scope of the claims and specification of the present application. In particular, as long as there is no structural conflict, the various technical features mentioned in the various embodiments can be combined in any way. The present application is not limited to the specific embodiments disclosed herein, but includes all technical solutions that fall within the scope of the claims.
Claims
1. A porous carbon material preparation device, characterized in that: include: A liquid nitrogen freezing container (100), wherein a freezing port (131) is provided on the top of the liquid nitrogen freezing container (100); A mold (200), wherein the mold (200) is arranged on the top of the liquid nitrogen freezing container (100), and the bottom of the mold (200) covers the freezing port (131), and the top of the mold (200) is provided with an air outlet (232) and an openable and closable air inlet (231); An elastic container (300) is used for being detachably connected to the air outlet (232).
2. The porous carbon material preparation device according to claim 1, characterized in that: The liquid nitrogen freezing container (100) comprises an inner shell (110), an outer shell (120) and an insulation layer (140); a first cavity for accommodating liquid nitrogen is formed inside the inner shell (110); the freezing port (131) is used to connect the inner and outer sides of the first cavity; the outer shell (120) is covered on the outside of the inner shell (110); and a closed second cavity is formed between the inner shell (110) and the outer shell (120); and the insulation layer (140) is filled in the second cavity.
3. The porous carbon material preparation device according to claim 2, characterized in that: The top surface of the liquid nitrogen freezing container (100) is further provided with a rib (132), the rib (132) surrounds the edge of the liquid nitrogen freezing container (100), and the top of the rib (132) is higher than the top surface of the liquid nitrogen freezing container (100).
4. The porous carbon material preparation device according to claim 1, characterized in that: The mold (200) comprises: a heat-insulating housing (210), wherein the top and bottom of the heat-insulating housing (210) are open; a heat-conducting base (220), the heat-conducting base (220) being used to be placed on the top of the liquid nitrogen freezing container (100), and the bottom of the heat-conducting base (220) completely covering the freezing port (131); the heat-insulating shell (210) being arranged on the top of the heat-conducting base (220) and being in sealed contact with the heat-conducting base (220); A heat-insulating sealing cover (230) is used to detachably seal the top of the heat-insulating shell (210), and the air inlet (231) and the air outlet (232) are arranged on the heat-insulating sealing cover (230).
5. The porous carbon material preparation device according to claim 4, characterized in that: A groove (221) is provided on the top of the heat-conducting base (220), and the bottom of the heat-insulating shell (210) is used to be inserted into the groove (221). When the bottom of the heat-insulating shell (210) is inserted into the groove (221), the outer side surface of the heat-insulating shell (210) is sealed and fitted with the inner side surface of the groove (221), and the bottom surface of the heat-insulating shell (210) is sealed and fitted with the bottom surface of the groove (221).
6. The porous carbon material preparation device according to claim 4, characterized in that: A detachable air inlet plug (420) is provided at the air inlet (231); when the air inlet plug (420) is inserted into the air inlet (231), the air inlet (231) is closed.
7. The porous carbon material preparation device according to claim 6, characterized in that: An air outlet plug (410) is provided at the air outlet (232), and a gas channel (411) is provided on the air outlet plug (410). The elastic container (300) is used to be detachably connected to the air outlet plug (410) and is in communication with the interior of the heat-insulating shell (210) through the gas channel (411).
8. The porous carbon material preparation device according to claim 7, characterized in that: The heat-insulating outer shell (210), the heat-insulating sealing cover (230), the air inlet plug (420), and the air outlet plug (410) are all made of polytetrafluoroethylene.
9. The porous carbon material preparation device according to claim 4, characterized in that: The heat-conducting base (220) is made of copper.
10. The porous carbon material preparation device according to claim 7, characterized in that: The elastic container (300) is a balloon.
Citation Information
Patent Citations
Automatic rapid freezing device based on ice template method
CN212619533U