Graphene microspheres and a preparation method thereof
By introducing a droplet size adjustment module into the graphene microsphere preparation device, the problem of inconvenient droplet size adjustment in the prior art is solved, and precise droplet adjustment and efficient molding are achieved, thereby improving the preparation efficiency of graphene microspheres.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- CHONGQING GRAPHENE RES INST CO LTD
- Filing Date
- 2023-12-15
- Publication Date
- 2026-06-05
AI Technical Summary
Existing graphene microsphere preparation devices cannot flexibly adjust the droplet size, requiring frequent replacement of the dropper, which is inconvenient to operate.
The droplet size adjustment module, including multi-layer adjustment units and control mechanism, is adopted. The droplet size is adjusted by the vertical movement of the control rod to achieve the step formation of droplets and improve the convenience of operation.
It achieves precise droplet control and high-quality molding, simplifies the operation process, and improves the preparation efficiency of graphene microspheres.
Smart Images
Figure CN117680035B_ABST
Abstract
Description
Technical Field
[0001] This invention relates to the field of microspheres, specifically to a graphene microsphere and its preparation method. Background Technology
[0002] Graphene microspheres can be filled into filter cartridges and adsorb pollutants in water to achieve the purpose of wastewater purification.
[0003] The existing method for preparing graphene microspheres includes the following steps: S1, preparation of graphene oxide material; S2, preparation of graphene oxide microsphere slurry; S3, preparation of graphene oxide gel microspheres; S4, curing and cleaning of graphene oxide gel microspheres; and S5, preparation of graphene microspheres.
[0004] S3 is carried out on a slurry extrusion device, through which graphene microsphere slurry can be extruded from a dropper. The extruded slurry exists in the form of droplets, which are similar to spheres. The droplets fall into the CaCl2 solution and are pre-cured to form graphene gel microspheres.
[0005] The size of the droplets determines the size of the microspheres, and the size of the droplets is mainly related to the size and specifications of the dropper. Currently, the slurry extrusion device cannot adjust the droplet size. If it is necessary to adjust the droplet size, it is also necessary to replace the dropper with a different size and specification. However, there are many droppers, and the droppers are located above the pre-curing tank. Replacing each dropper one by one requires very little manual operation space, which is very inconvenient. Summary of the Invention
[0006] The present invention aims to provide a graphene microsphere and a method for preparing the same, so as to facilitate the adjustment of the size of the prepared microsphere.
[0007] To achieve the above objectives, the present invention adopts the following technical solution: a method for preparing graphene microspheres, comprising a step of preparing droplets of graphene microsphere slurry, wherein the droplets of graphene microsphere slurry are dripped out through a dropper, the bottom of the dropper is provided with a droplet size adjustment module, the droplet size adjustment module includes multiple adjustment units, each adjustment unit is provided with a forming droplet hole, the forming droplet holes on the multiple adjustment units are vertically opposite each other, the diameter of the forming droplet holes on each adjustment unit gradually decreases from top to bottom, and the inner walls of multiple forming droplet holes form a stepped hole; each adjustment unit includes two horizontally sliding adjustment plates, the ends of the two adjustment plates are opposite each other, the opposite ends of the two adjustment plates are provided with arc-shaped grooves, when the two adjustment plates abut against each other, the arc-shaped grooves are opposite each other and form a forming droplet hole;
[0008] The droplet size adjustment module also includes a control mechanism for controlling the opening and closing states of each adjustment unit;
[0009] When it is necessary to adjust the size of the droplets, the size of the droplets can be adjusted by controlling the opening and closing state of each layer of adjustment unit. When all layers of adjustment units are closed, the droplets are the smallest. From bottom to top, as the number of layers of adjustment units that are open gradually increases, the droplets gradually become larger.
[0010] The principle and advantages of this scheme are as follows: In this scheme, the diameter of the forming droplets on each layer of the adjustment unit gradually decreases from top to bottom, and the inner walls of multiple forming droplets form a stepped shape, thus forming a stepped hole. When the droplets flow downward in the forming droplets, because the diameter of multiple forming droplets gradually decreases from top to bottom, compared to the diameter of multiple forming droplets gradually increasing from top to bottom, the stepped hole gradually shrinks from top to bottom. As the slurry flows downward, it will gradually gather towards the center, making it easier for the droplets to form spherical shapes. The droplets are more rounded, and the final microspheres are of higher quality.
[0011] In this scheme, the size of the droplet formation is related to the size of the forming orifice of the bottommost closed adjustment unit. That is, regardless of the number of adjustment units, the larger the forming orifice of the bottommost closed adjustment unit (when the two adjustment plates are in contact), the larger the final droplet will be; conversely, the smaller the forming orifice of the bottommost closed adjustment unit, the smaller the final droplet will be. Therefore, by controlling the opening and closing of the adjustment units through a control mechanism, the size of the droplet can be changed, thus changing the size of the microspheres. This allows for application in different filter cartridges. In this way, during the preparation of graphene microspheres, there is no need to manually replace the dropper to change the size of the liquid, greatly improving operational convenience.
[0012] Therefore, with this solution, to form droplets of the corresponding size, it is only necessary to close the adjustment unit of the corresponding layer forming the droplet of that size and open the adjustment unit below that layer. The opening and closing of the adjustment unit above that layer is not significantly related to the size of the droplet. However, if the adjustment unit above that layer is open, it is impossible to form a stepped aperture that is wider at the top and narrower at the bottom, thus failing to restrict the droplet formation and failing to achieve the effect that "the stepped aperture makes it easier for the droplet to form a spherical shape, and the droplet is more round." Therefore, in this solution, when adjusting the droplet from small to large, the adjustment units are opened layer by layer from the bottom to the top, thus making the droplet gradually larger. When adjusting the droplet from large to small, the adjustment units are closed layer by layer from the top to the bottom, thus making the droplet gradually smaller. By operating in this order, it can be ensured that when the adjustment unit for forming the droplet size is in the closed state, the adjustment unit below this layer of adjustment unit is in the open state, and all the adjustment units above this layer of adjustment unit are also in the closed state. This results in multiple forming droplet holes forming a stepped hole that is wider at the top and narrower at the bottom, ensuring that the droplet shape is better and closer to a sphere.
[0013] Preferably, as an improvement, the control mechanism includes a control lever and a drive component for vertically moving the control lever, with the control lever abutting against the end of the adjusting plate; the control lever is vertically arranged and includes an upper section and a lower section, with the upper section located above the lower section, the lateral distance from the upper section to the dropper being less than the lateral distance from the lower section to the dropper, and an inclined section connecting the upper and lower sections; an elastic unit is connected to the adjusting plate, and the elastic unit exerts a force on the adjusting plate to move the adjusting plate closer to the lower section;
[0014] The control lever is moved vertically by the drive component. When the control lever moves vertically upward, the adjustment unit opens layer by layer from bottom to top. When the control lever moves vertically downward, the adjustment unit closes layer by layer from top to bottom.
[0015] Therefore, the drive component drives the control lever to move vertically. When the upper section of the control lever abuts against the ends of the adjustment plates of all layers, the adjustment units of all layers are in the closed state. As the control lever gradually moves upward, the adjustment plates of the adjustment units of each layer from bottom to top gradually detach from the upper section. The ends of the adjustment plates no longer abut against the upper section. After the adjustment plates detach from the upper section, the two adjustment plates of each layer move away from each other under the action of the elastic unit. The adjustment plates move laterally towards the inclined section and even laterally towards the lower section, so that the two adjustment plates no longer abut against each other, and the adjustment unit opens. Thus, as the control lever gradually moves upward, the adjustment units of each layer from bottom to top gradually open, and the formed droplets gradually become larger.
[0016] Conversely, when the control lever moves downwards, the ends of the adjustment plates of the adjustment units that open from top to bottom gradually move through the inclined section to the upper section and abut against it. Under the pressure of the upper section, the adjustment plates overcome the elastic force of the elastic unit and move, bringing the two adjustment plates closer together and abutting against each other, thus closing the adjustment unit. Therefore, as the control lever moves downwards, the adjustment units that open from top to bottom gradually close, and the formed droplets gradually become smaller.
[0017] Therefore, by moving the control rod vertically in this scheme, the adjustment units of each layer can be opened or closed sequentially, without any problem of incorrect opening or closing order of the adjustment units. This ensures that the forming orifices of multiple adjustment units in the closed state form stepped orifices, thus guaranteeing the forming quality of the droplets.
[0018] In addition, the inclined section in this design serves as a transition between the upper and lower sections, and the end of the adjustment plate will not get stuck when switching between the upper and lower sections.
[0019] Preferably, as an improvement, the driving component includes a fine-tuning motor and a fine-tuning screw, the fine-tuning motor and the fine-tuning screw are coaxially connected, and a moving block is fixedly connected to the control rod, the moving block and the fine-tuning screw are threadedly connected;
[0020] The vertical movement of the control lever is controlled by adjusting the fine-tuning motor.
[0021] Therefore, by rotating the fine-tuning screw via the fine-tuning motor, the fine-tuning screw moves the moving block, thus achieving the vertical movement of the control lever. This adjustment method offers higher precision and is suitable for adjusting smaller displacements.
[0022] Preferably, as an improvement, the number of layers in the adjustment unit is 6-10. Therefore, controlling the number of layers within this range is more appropriate.
[0023] Preferably, as an improvement, the method further includes a step of preparing graphene oxide gel microspheres, wherein the formed droplets fall downwards into a pre-curing tank for pre-curing to form graphene oxide gel microspheres, and gas is passed upwards through the interior of the pre-curing tank.
[0024] Thus, the droplets falling into the pre-curing tank undergo pre-curing in the calcium chloride solution, forming graphene oxide gel microspheres. During the pre-curing process, gas is circulated upwards inside the pre-curing tank, which provides resistance to the droplet's fall, reduces the droplet's downward velocity, and prevents the droplets from accumulating at the bottom of the pre-curing tank. This facilitates full contact between the droplets and the calcium chloride solution in the pre-curing tank, improving the pre-curing effect and resulting in better droplet solidification.
[0025] Preferably, as an improvement, it further includes a graphene oxide gel microsphere curing step, wherein the pre-curing pool is inclined, the lower end of the pre-curing pool is provided with a curing pool, and the top of the pre-curing pool and the top of the curing pool are connected;
[0026] The pre-cured droplets in the pre-curing tank automatically flow downwards into the curing tank for curing for 12-24 hours.
[0027] Therefore, the pre-cured graphene oxide gel microspheres flow along the inclined liquid surface into the curing tank. Since there is no upward blowing gas in the curing tank, the graphene oxide gel microspheres will deposit in the curing tank for a long time to cure. Because the curing time in the curing tank is relatively long, the deposition and aggregation of the graphene oxide gel microspheres in the curing tank also ensures that they are fully cured.
[0028] Since the graphene oxide gel microspheres need to flow downwards into the curing tank, the upward blowing gas in the pre-curing tank can prevent the graphene oxide gel microspheres from sinking to the bottom, which is conducive to the graphene oxide gel microspheres flowing from the upper part of the pre-curing tank into the curing tank.
[0029] Preferably, as an improvement, the curing tank is equipped with a retrieval box. After curing is completed, the retrieval box retrieves the cured graphene oxide gel microspheres from the curing tank and washes them with deionized water.
[0030] In this method, graphene oxide gel microspheres are deposited in a curing tank and then transferred to a retrieval box. After curing, the microspheres are retrieved from the curing tank by lifting the retrieval box. In this method, the graphene oxide gel microspheres enter the curing tank from the top under the influence of gas, which facilitates their entry into the retrieval box. If the microspheres enter the curing tank from the bottom of the pre-curing tank, they are less likely to enter the retrieval box.
[0031] Preferably, as an improvement, the method further includes the following steps: after washing the graphene oxide gel microspheres, the graphene oxide microsphere gel is placed in a Teflon hydrothermal reactor, and then placed in an oven at 80-200℃ for 12-24 hours. This achieves the reduction of the graphene oxide microspheres.
[0032] Preferably, as an improvement, the method further includes the following steps: the product prepared in the Teflon hydrothermal reactor is washed multiple times in an ethanol solution, then washed multiple times with deionized water, and finally freeze-dried. This thoroughly cleans the reactants adsorbed by the graphene microspheres during the hydrothermal reaction, resulting in a cleaner surface and better adsorption properties for the prepared microspheres.
[0033] To achieve the above objectives, the present invention employs the following technical solution: a graphene microsphere, prepared by the above method. Any graphene microspheres prepared using the preparation method of the present invention are also protected by this patent. Attached Figure Description
[0034] Figure 1 This is a schematic diagram of the apparatus for preparing graphene microspheres.
[0035] Figure 2 for Figure 1 A magnified view of A in the middle.
[0036] Figure 3 for Figure 1 A magnified view of B in the middle.
[0037] Figure 4 A schematic diagram of the structure for controlling and driving the control lever using a drive component.
[0038] Figure 5 This is a top view of the adjustment unit in one of the layers. Detailed Implementation
[0039] The following detailed description illustrates the specific implementation method:
[0040] The reference numerals in the accompanying drawings include: slurry tank 1, piston plate 2, feed pipe 3, electrically controlled feed valve 4, drip pipe 5, electrically controlled discharge valve 6, funnel section 7, pre-curing tank 8, vent pipe 9, notch 10, retrieval box 11, curing tank 12, retrieval rope 13, adjusting plate 14, upper section 15, fine-tuning motor 16, moving block 17, fixed block 18, compression spring 19, guide rod 20, slide plate 21, frame 22, forming drip hole 23, lower section 24, fine-tuning screw 25.
[0041] The basic implementation examples are as follows: Figures 1-5 As shown: A method for preparing graphene microspheres includes the following steps:
[0042] S1. Graphene oxide was prepared using the Hummers method.
[0043] S2. Prepare a 0.6% (w / w) solution of graphene oxide and add 1% (w / w) sodium alginate. Stir well and heat at 50-60°C for 1-2 hours, then cool.
[0044] S3. Preparation of graphene microsphere slurry droplets, performed on a graphene microsphere preparation device. Combined with... Figure 1 As shown, the graphene microsphere fabrication apparatus includes a frame ( Figure 1 (Not shown) and a slurry tank 1, which is bolted to the frame. Inside the slurry tank 1 is a piston plate 2, horizontally positioned and vertically slidably connected to the inner wall of the slurry tank 1. A drive rod is bolted to the top of the piston plate 2. A drive component is bolted to the frame, connected to the drive rod. The drive component allows the drive rod to move vertically, thus moving the piston plate 2 up and down. The drive component can be a pneumatic cylinder or a hydraulic cylinder, or a motor combined with a screw can be used to drive the drive rod vertically.
[0045] A feed pipe 3 is connected to the side wall of the slurry tank 1, and an electrically controlled feed valve 4 is installed on the feed pipe 3. Multiple droppers 5 are installed at the bottom of the slurry tank 1, and each dropper 5 is connected to an electrically controlled discharge valve 6. In this embodiment, three droppers 5 are shown for illustration; however, in actual use, more can be used, such as 10 or 20.
[0046] The bottom of each dropper 5 has a funnel-shaped section 7, which is wider at the top and narrower at the bottom, allowing the liquid to collect as it flows from top to bottom through the dropper 5. Each dropper 5 also has a droplet size adjustment module at its bottom, which, combined with... Figure 2As shown, the droplet size adjustment module includes multiple adjustment units. In this embodiment, there are six adjustment units, but in other embodiments, there can be 7-10 layers. Each layer of the adjustment unit is provided with a forming droplet hole 23. The forming droplet holes 23 on the multiple adjustment units are vertically opposite each other, and the diameter of the forming droplet holes 23 on each layer of the adjustment unit gradually decreases from top to bottom. In this way, the inner walls of multiple forming droplet holes 23 form a stepped shape, and multiple forming droplet holes 23 form a stepped hole with a larger diameter at the top and a smaller diameter at the bottom. Combined with Figure 2 and Figure 5 As shown, each adjustment unit includes two laterally sliding adjustment plates 14. A sliding plate 21 is welded to the side of each adjustment plate 14, and the sliding plate 21 is laterally slidably connected to the frame 22. The ends of the two adjustment plates 14 face each other, and arc-shaped grooves are provided on the opposite ends of the two adjustment plates 14. When the two adjustment plates 14 abut, the arc-shaped grooves align and form a shaped drip hole 23. Since the diameter of the shaped drip hole 23 in the upper adjustment unit is larger than the diameter of the shaped drip hole 23 in the lower adjustment unit, the diameter of the arc-shaped groove in the upper adjustment plate 14 is larger than the diameter of the arc-shaped groove in the lower adjustment plate 14.
[0047] The droplet size adjustment module in this embodiment also includes a control mechanism for controlling the opening and closing states of each adjustment unit. The control mechanism includes a control lever and a drive component for vertically moving the control lever. Combined with... Figure 3 and Figure 4 As shown, each dropper 5 has two control levers and two drive components on each side. The left control lever abuts against the left end of the left adjustment plate 14, and the right control lever abuts against the right end of the right adjustment plate 14. In this embodiment, the control levers are vertically arranged and include an upper section 15 and a lower section 24. The upper section 15 is located above the lower section 24, and the distance from the upper section 15 to the dropper 5 is less than the distance from the lower section 24 to the dropper 5. An inclined section connects the upper section 15 and the lower section 24. Figure 3 As shown, the distance between the left side wall of the upper section 15 and the left side wall of the lower section 24 of the right-side control lever is the distance that the right-side adjustment plate 14 slides to the right. In this embodiment, the two control levers, the two drive components, and the adjustment plates 14 on both sides are all symmetrically arranged about the vertical axis of the dropper 5.
[0048] Combination Figure 5As shown, an elastic unit is connected to the adjusting plate 14. The elastic unit exerts a force on the adjusting plate 14, causing it to move towards the lower section 24. In this embodiment, the elastic unit includes a fixing block 18 located on the side of the adjusting plate 14. A fixing block 18 is welded to the side of each adjusting plate 14. A transverse guide rod 20 is welded to the fixing block 18 on the right adjusting plate 14. The guide rod 20 passes through the fixing block 18 on the left adjusting plate 14 and slides laterally with the fixing block 18 on the left adjusting plate 14. A compression spring 19 connects the fixing blocks 18 on the left and right adjusting plates 14, and the compression spring 19 is sleeved on the guide rod 20. Thus, the two adjusting plates 14 tend to move away from each other under the action of the compression spring 19.
[0049] Each control lever is connected to a drive component. In this embodiment, the drive component includes a fine-tuning motor 16 and a fine-tuning screw 25. The fine-tuning electrode is bolted to the frame 22. The fine-tuning motor 16 and the fine-tuning screw 25 are coaxially fixedly connected. A moving block 17 is welded to the control lever, and the fine-tuning screw 25 passes through the moving block 17. The moving block 17 and the fine-tuning screw 25 are threadedly connected. Thus, by controlling the fine-tuning motor 16, the fine-tuning screw 25 is rotated. The fine-tuning screw 25 drives the moving block 17 to move vertically, thereby driving the vertical movement of the control lever. In this embodiment, the control lever and the moving block 17 are vertically slidably connected to the frame 22. Specifically, the frame 22 is provided with a vertical T-shaped groove. Both the control lever and the moving block 17 are integrally connected to a sliding part, which slides within the T-shaped groove. This arrangement makes the vertical movement of the control lever more stable.
[0050] In this embodiment, as Figure 3 In the state shown, the two adjusting plates 14 on all adjusting units are abutted by the upper sections 15 of the control rods on both sides, and the two adjusting plates 14 on all adjusting units are in a mutually abutting state. At this time, the forming drip hole 23 is formed as shown. Figure 2 The stepped hole shown.
[0051] In use, the electrically controlled feed valve 4 is opened and the electrically controlled discharge valve 6 is closed. Then, the piston plate 2 is moved upward, creating a negative pressure in the slurry tank 1. The slurry prepared in S2 enters the slurry tank 1 through the feed pipe 3. Then, the electrically controlled feed valve 4 is closed and the electrically controlled discharge valve 6 is opened, causing the piston plate 2 to move slowly downward. The piston plate 2 slowly squeezes the slurry in the slurry tank 1 downward, and the slurry enters the dropper 5. The slurry flows downward through the multi-layer forming droplet holes 23, and drips out from the forming droplet holes 23 of the lowest adjustment unit to form droplets. The droplets continuously drip downward, thus realizing the preparation of graphene microsphere slurry droplets. In this embodiment... Figure 2The diameter of the bottom forming dropper 23 is 0.8 mm, and the diameter of the top forming dropper 23 is 3.3 mm.
[0052] In this embodiment, the size of the droplet is related to the size of the forming orifice 23 of the adjustment unit at the bottom, which is in the closed state. The diameter of the droplet is adjusted from 1 to 4 mm. When it is necessary to increase the size of the droplet, the fine-tuning motor 16 drives the fine-tuning screw 25 to rotate, the fine-tuning screw 25 drives the moving block 17 to move upward, and the moving block 17 drives the control lever to move upward. Figure 3 As shown, the end of the adjusting plate 14 of the lowest adjusting unit will disengage from the upper section 15, and the end of the adjusting plate 14 of the lowest adjusting unit will be freed from the pressure of the upper section 15. The end of the adjusting plate 14 of the lowest adjusting unit will be opposite to the inclined section. At this time, the two adjusting plates 14 of the lowest adjusting unit will move away from each other under the action of the compression spring 19, and the two adjusting plates 14 of the lowest adjusting unit will no longer be pressed together, thus making the lowest adjusting unit open, while the adjusting unit of the second layer below will remain closed. At this time, the droplet will be formed under the action of the forming droplet hole 23 of the second layer below. Since the forming droplet hole 23 of the second layer below has a larger aperture than the forming droplet hole 23 of the lowest layer, the droplet will also become larger. Similarly, as the control lever continues to move upward, the adjusting unit of the second layer below will open, and the forming droplet hole 23 on the adjusting unit of the third layer below will play a role in the formation of the droplet, and the droplet will become larger. In this way, as the control lever continues to move upward, the adjusting units will open layer by layer from bottom to top, and the volume of the droplet will continuously increase.
[0053] When it is necessary to reduce the size of the droplet, the drive control lever moves downward. The end of the adjustment plate 14 of the adjustment unit, which is in the open state, gradually slides from the inclined section to the upper section 15. The upper section 15 presses against the end of the adjustment plate 14 that has slid to the upper section 15, causing the two adjustment plates 14 on the adjustment unit to overcome the elastic force of the compression spring 19 and move closer to each other. The ends of the two adjustment plates 14 abut against each other, thereby closing the adjustment unit. Compared with the lowermost forming droplet orifice 23 before adjustment, a smaller forming droplet orifice 23 is formed, making the droplet smaller. Thus, as the control lever continues to move downward, the adjustment unit closes layer by layer from top to bottom, and smaller forming droplet orifices 23 are continuously formed, thereby continuously reducing the volume of the droplet.
[0054] S4. Preparation of graphene oxide gel microspheres. The graphene microsphere preparation apparatus in this embodiment also includes a pre-curing tank 8, located below the dropper 5. The pre-curing tank 8 is inclined, and multiple air outlet pipes 9 are provided at the bottom of the pre-curing tank 8. The pre-curing tank 8 contains a calcium chloride solution (mass fraction 10-15%).
[0055] The resulting droplets fall downwards into the pre-curing tank 8 for pre-curing to form graphene oxide gel microspheres. Gas is introduced upwards into the pre-curing tank 8. The gas slows down the downward movement of the droplets, preventing them from settling and accumulating at the bottom, which is beneficial for the formation of graphene oxide gel microspheres in the upper part of the pre-curing tank 8.
[0056] S5. Curing of graphene oxide gel microspheres. A curing tank 12 is provided at the lower end of the pre-curing tank 8. A baffle is provided between the pre-curing tank 8 and the curing tank 12, and a notch 10 is provided at the top of the baffle, thereby connecting the top of the pre-curing tank 8 and the top of the curing tank 12. As a result, the graphene oxide gel microspheres formed in the pre-curing tank 8 enter the curing tank 12 along the inclined surface and sink to the bottom of the curing tank 12. A retrieval box 11 is provided in the curing tank 12. The retrieval box 11 has filter holes (the pore size of the filter holes is smaller than the diameter of the graphene oxide gel microspheres). The graphene oxide gel microspheres that sink to the bottom of the curing tank 12 enter the retrieval box 11.
[0057] In this step, the graphene oxide gel microspheres are cured in curing tank 12 for 12-24 hours.
[0058] After curing, the cured graphene oxide gel microspheres in the retrieval box 11 are retrieved from the curing pool 12 by the retrieval rope 13 and then washed with deionized water.
[0059] S6. After washing the graphene oxide gel microspheres, place the graphene oxide microsphere gel in a Teflon hydrothermal reactor with a filling volume of 60-70%, and then place it in an oven at 80-200℃ for 12-24 hours. This achieves the reduction of graphene oxide microspheres.
[0060] S6. The product prepared in the Teflon hydrothermal reactor is washed multiple times in ethanol solution, then washed multiple times with deionized water, and finally freeze-dried to obtain graphene microspheres.
[0061] The above descriptions are merely embodiments of the present invention, and common knowledge such as specific technical solutions and / or characteristics are not described in detail here. It should be noted that those skilled in the art can make various modifications and improvements without departing from the technical solutions of the present invention, and these should also be considered within the scope of protection of the present invention. These modifications and improvements will not affect the effectiveness of the implementation of the present invention or the practicality of the patent. The scope of protection claimed in this application should be determined by the content of its claims, and the specific embodiments described in the specification can be used to interpret the content of the claims.
Claims
1. A method for preparing graphene microspheres, comprising a droplet preparation step of graphene microsphere slurry, wherein, The graphene microsphere slurry is dispensed as droplets through a dropper, characterized in that: the bottom of the dropper is provided with a droplet size adjustment module, the droplet size adjustment module includes multiple adjustment units, each adjustment unit is provided with a forming droplet hole, the forming droplet holes on the multiple adjustment units are vertically opposite each other, the diameter of the forming droplet holes on each adjustment unit gradually decreases from top to bottom, and the inner walls of multiple forming droplet holes form a stepped hole; each adjustment unit includes two horizontally sliding adjustment plates, the ends of the two adjustment plates are opposite each other, the opposite ends of the two adjustment plates are provided with arc-shaped grooves, when the two adjustment plates abut against each other, the arc-shaped grooves are aligned and form the forming droplet hole; The droplet size adjustment module also includes a control mechanism for controlling the opening and closing states of each adjustment unit; When it is necessary to adjust the size of the droplets, the size of the droplets can be adjusted by controlling the opening and closing state of each layer of adjustment unit; when all layers of adjustment units are closed, the droplets are the smallest; from bottom to top, as the number of layers of adjustment units that are open gradually increases, the droplets gradually become larger. The control mechanism includes a control rod and a drive component for vertically moving the control rod, with the control rod abutting against the end of the adjusting plate. The control rod is vertically oriented and includes an upper section and a lower section, with the upper section located above the lower section. The lateral distance from the upper section to the dropper is less than the lateral distance from the lower section to the dropper. An inclined section connects the upper and lower sections. An elastic unit is connected to the adjusting plate, and the elastic unit exerts a force on the adjusting plate to move it closer to the lower section. The control lever is moved vertically by the drive component. When the control lever moves vertically upward, the adjustment unit opens layer by layer from bottom to top. When the control lever moves vertically downward, the adjustment unit closes layer by layer from top to bottom.
2. The method for preparing graphene microspheres according to claim 1, characterized in that: The driving component includes a fine-tuning motor and a fine-tuning screw, the fine-tuning motor and the fine-tuning screw are coaxially connected, and a moving block is fixedly connected to the control rod, the moving block and the fine-tuning screw are threadedly connected; The vertical movement of the control lever is controlled by adjusting the fine-tuning motor.
3. The method for preparing graphene microspheres according to claim 1, characterized in that: The adjustment unit has 6-10 layers.
4. The method for preparing graphene microspheres according to claim 1, characterized in that: It also includes a step of preparing graphene oxide gel microspheres, wherein the formed droplets fall downwards into a pre-curing tank for pre-curing to form graphene oxide gel microspheres, and gas is passed upwards through the interior of the pre-curing tank.
5. The method for preparing graphene microspheres according to claim 4, characterized in that: It also includes a graphene oxide gel microsphere curing step, wherein the pre-curing pool is inclined, the lower end of the pre-curing pool is provided with a curing pool, and the top of the pre-curing pool and the top of the curing pool are connected. The pre-cured droplets in the pre-curing tank automatically flow downwards into the curing tank for curing for 12-24 hours.
6. The method for preparing graphene microspheres according to claim 5, characterized in that: The curing tank is equipped with a retrieval box. After curing is complete, the retrieval box retrieves the cured graphene oxide gel microspheres from the curing tank and washes them with deionized water.
7. The method for preparing graphene microspheres according to claim 6, characterized in that: It also includes the following steps: After washing the graphene oxide gel microspheres, place the graphene oxide microsphere gel in a Teflon hydrothermal reactor, and then place it in an oven to react at 80-200℃ for 12-24 hours.
8. The method for preparing graphene microspheres according to claim 7, characterized in that: It also includes the following steps: The product prepared in a Teflon hydrothermal reactor is washed multiple times in an ethanol solution, then washed multiple times with deionized water, and finally freeze-dried.