CN111620328A - Large-scale graphene preparation process - Google Patents
Large-scale graphene preparation process Download PDFInfo
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- CN111620328A CN111620328A CN202010459451.7A CN202010459451A CN111620328A CN 111620328 A CN111620328 A CN 111620328A CN 202010459451 A CN202010459451 A CN 202010459451A CN 111620328 A CN111620328 A CN 111620328A
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- C01—INORGANIC CHEMISTRY
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- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/184—Preparation
- C01B32/19—Preparation by exfoliation
- C01B32/192—Preparation by exfoliation starting from graphitic oxides
Abstract
The invention discloses a large-scale graphene preparation process in the technical field of graphite preparation, which comprises the following steps: the method comprises the following steps: oxidizing graphite powder by concentrated sulfuric acid and potassium permanganate to prepare graphite oxide, and performing vacuum drying on the prepared graphite oxide; according to the invention, the grinding motor, the grinding shaft, the first grinding roller, the grinding tank body, the fixing plate, the U-shaped filter plate, the collecting hopper, the T-shaped frame, the conveying pipe, the communicating pipe, the conveying motor, the conveying shaft, the conveying leaves, the collecting hopper, the driving gear, the follow-up fluted disc and the linkage rod are arranged, so that the grinding, screening and re-grinding work is automatically completed in one grinding device, the working processes are closely linked, separate operation is not needed, the time of manual transfer operation is saved, the working efficiency is improved, and the working progress of preparing graphene is ensured.
Description
Technical Field
The invention relates to the technical field of graphite preparation, in particular to a large-scale graphene preparation process.
Background
Graphene is a single-layer graphite sheet having a two-dimensional ordered structure, which exists alone, and graphene oxide is an oxide of graphene.
The prior art discloses an invention case of a partial graphene preparation process, and a Chinese patent with the patent application number of 201810568818.1 discloses a large-scale graphene preparation process, which comprises the following steps: taking natural flake graphite or artificial graphite as a raw material, firstly adding an oxidant for oxidation reaction to prepare graphite oxide, then adding an intercalation agent for intercalation reaction, and after the intercalation reaction is finished, carrying out suction filtration on a reaction solution to obtain dried intercalated graphite; grinding and sieving the prepared dried intercalated graphite by using grinding equipment to obtain expandable graphite; dispersing the obtained expandable graphite in an ultrasonic treatment solvent, and carrying out ultrasonic treatment to realize primary stripping; and (3) primarily stripping graphite from the obtained ultrasonic waves, and mixing concentrated sulfuric acid and graphite by using graphene production equipment to realize final stripping to obtain graphene.
In the process of preparing graphene in the prior art, more particles with unsatisfactory particle size exist in the particle fineness of graphite oxide obtained by grinding graphite oxide, a large amount of graphite oxide meeting the ideal fineness needs to be ground, so that the graphite oxide particles which are not satisfactory after being ground by a single time need to be ground by a worker again, and then a screening program is used for screening, so that the whole operation process needs manual transfer and is troublesome, the working efficiency is too low, and the preparation progress of the whole preparation process is influenced.
Based on the above, the invention designs a large-scale graphene preparation process to solve the above problems.
Disclosure of Invention
The invention aims to provide a large-scale graphene preparation process, and aims to solve the problems that in the prior art, in the process of preparing graphene, more particles with unsatisfactory particle size exist in the particle fineness of graphite oxide obtained by grinding graphite oxide, and a large amount of graphite oxide needs to be ground to generate graphite oxide meeting the ideal fineness, so that the graphite oxide particles which are not satisfactory in single grinding are ground again by workers and then screened by a screening program, the whole operation process needs manual transfer, is troublesome, the working efficiency is too low, and the preparation progress of the whole preparation process is influenced. To a problem of (a).
In order to achieve the purpose, the invention provides the following technical scheme: a large-scale graphene preparation process comprises the following steps:
the method comprises the following steps: oxidizing graphite powder by concentrated sulfuric acid and potassium permanganate to prepare graphite oxide, and performing vacuum drying on the prepared graphite oxide;
step two: putting the graphite oxide after vacuum drying into grinding equipment for grinding, and then directly screening, wherein the graphite oxide is ground into particles of more than 300 meshes;
step three: putting the graphite oxide particles obtained by screening into a mixing container, adding ionized water according to the proportion that 300mg of graphite oxide particles are dispersed in 60ml of ionized water, and mixing by ultrasonic vibration to obtain colloidal suspension;
step four: then transferring the colloidal suspension into a stirring container, adding sodium borohydride and sodium dodecyl benzene sulfonate, heating to 80 ℃, refluxing for 16h under the condition, performing centrifugal separation, sequentially washing with acetone and deionized water until the pH value is 7, and performing vacuum drying on the obtained filter cake to obtain graphene;
wherein, in the second step, the grinding device comprises a grinding shell, the two sides of the top of the grinding shell are fixedly communicated with feed hoppers, the middle position of the top of the grinding shell is fixedly connected with a grinding motor, the output end of the grinding motor is fixedly connected with a grinding shaft, the bottom end of the grinding shaft penetrates into the grinding shell and is fixedly connected with a first grinding roller, the inner wall of the grinding shell is fixedly connected with a grinding groove body which is matched and ground with the first grinding roller, the top end of the inner wall of the grinding groove body is provided with an inclined arc surface, the bottom of the grinding groove body is fixedly connected with a discharge hopper, the lower surface of the grinding shell is fixedly connected with a fixed plate, the four corners of the bottom of the fixed plate are fixedly connected with supporting legs, the bottoms of the four supporting legs are fixedly connected with a base, the side surface of the fixed plate is connected with a backflow conveying mechanism for backflow of the grinding particles into the grinding shell, and the backflow conveying mechanism shakes the grinding particle screening mechanism back and forth through a linkage mechanism;
the grinding particle screening mechanism comprises an obliquely arranged U-shaped filter plate, the lower end of the U-shaped filter plate is fixedly connected with a return hopper, the bottom of the U-shaped filter plate is fixedly connected with a collecting hopper which is obliquely arranged in the opposite direction, two sides of the U-shaped filter plate and the collecting hopper are both fixedly connected with two supporting plates together, the bottoms of the two supporting plates on the same side are fixedly connected with sliding blocks together, the top of the base is fixedly connected with a sliding rail corresponding to the position of the sliding block, the sliding block is connected onto the surface of the sliding rail in a sliding manner, and a T-shaped frame is fixedly connected between;
the backflow conveying mechanism comprises a conveying pipe which is fixedly connected with the side surface of the fixing plate, the top end of the side surface of the conveying pipe is fixedly communicated with an obliquely arranged communicating pipe, one end of the communicating pipe, which is far away from the conveying pipe, is communicated with the top end of the side surface of the grinding shell, the top of the conveying pipe is fixedly connected with a conveying motor, the output end of the conveying motor is fixedly connected with a conveying shaft, the bottom end of the conveying shaft penetrates into the conveying pipe and is fixedly connected with a conveying blade on the surface, the bottom end of the conveying shaft is rotatably connected to the top of the base, the surface of the conveying shaft is rotatably connected with a material collecting hopper, the side surface of the collecting hopper is fixedly connected with a connecting seat which is fixedly connected with the side surface of the base, the bottom end of the conveying pipe is positioned in the collecting hopper and close to the bottom of the inner wall of the collecting hopper, and the end part of the discharging hopper extends to the position, close to the conveying pipe, of the top of the collecting hopper;
the linkage mechanism comprises a driving gear and a follow-up fluted disc, the driving gear is fixedly connected to the surface of the conveying shaft and is positioned below the collecting hopper, the follow-up fluted disc is rotatably connected to the top of the base, the follow-up gear is positioned between the driving gear and the T-shaped frame, the side surface of the follow-up gear is meshed with the side surface of the driving gear, the left side of the top of the follow-up gear is fixedly connected with a first connecting shaft, the left end of the T-shaped frame is fixedly connected with a second connecting shaft, and the surfaces of the second connecting shaft and the first connecting shaft are jointly and rotatably connected with a linkage;
during operation, the graphite oxide particles with unsatisfactory particle size are obtained by grinding the graphite oxide, a large amount of graphite oxide meeting the ideal fine mesh needs to be ground, so that a worker needs to grind the graphite oxide particles which are not satisfactory after single grinding again, and then the graphite oxide particles are screened by a screening program, the whole operation process needs manual transfer and is troublesome, the working efficiency is too low, and the preparation progress of the whole preparation process is influenced, the grinding, screening and re-grinding projects are completed on one device by arranging a first grinding roller, a grinding groove body, a grinding particle screening mechanism, a backflow conveying mechanism and a linkage mechanism, a grinding motor and a conveying motor are started by an external controller, then the larger graphite oxide is broken and put into a grinding shell through a feed hopper, and the grinding motor drives the first grinding roller to rotate through a grinding shaft, the first grinding roller can extrude graphite oxide into a position between the first grinding roller and a grinding groove body for grinding, the graphite oxide particles after grinding can be shunted to the inside of a U-shaped filter plate through a discharge hopper for screening, the screening fine meshes of the U-shaped filter plate are meshes, meanwhile, a conveying motor drives a conveying blade and a driving gear to rotate through a conveying shaft, the driving gear drives a follow-up fluted disc to rotate, the follow-up fluted disc is linked with a T-shaped frame back and forth through a linkage rod, the T-shaped frame is driven by a sliding block and a supporting plate to pull the U-shaped filter plate and a collecting hopper to shake, the graphite oxide particles passing through the U-shaped filter plate are more than meshes, the preparation requirements are met, the graphite oxide particles are collected by the collecting hopper and are drained out for direct use, meanwhile, the larger graphite oxide particles screened out can be drained to the inside of the collecting hopper through a backflow hopper, under the conveying action of the conveying blade, the larger graphite oxide particles are vertically, the secondary grinding is carried out, the whole process does not need manual operation, the grinding, screening and secondary grinding work is automatically completed in one grinding device, the working processes are closely linked, separate operation is not needed, the time of manual transfer operation is saved, the working efficiency is improved, and the working progress of preparing graphene is ensured; the inclined arc surface is arranged at the top end of the inner wall of the grinding groove body, so that the introduced graphite oxide fragments or the returned oxidized particles are drained, and the graphite oxide fragments or the returned oxidized particles enter a gap between the first grinding roller and the grinding groove body.
As a further scheme of the invention, a connecting frame is fixedly connected to the surface of the grinding shaft and positioned inside the grinding shell, a second grinding roller is rotatably connected to the end part of the connecting frame far away from the grinding shaft, an annular inclined plane is arranged at the left end of the second grinding roller, and the surface of the second grinding roller is in contact with an inclined arc surface at the top of the inner wall of the grinding groove body; during operation, the graphite oxide fragments or the reflowing oxidized particles can not enter the grinding gap between the first grinding roller and the grinding groove quickly, can be stacked together and can not be dispersed, and can also cause overstock plugging to the inlet of the first grinding roller and the grinding groove gap, through arranging the second grinding roller, the grinding shaft can drive the second grinding roller to roll along the inclined arc surface at the top of the inner wall of the grinding groove body, the graphite oxide fragments or the reflowing oxidized particles on the inclined arc surface are rolled in advance, the fineness of the graphite oxide fragments or the reflowing oxidized particles is reduced, so that the graphite oxide fragments or the reflowing oxidized particles can enter the grinding gap between the first grinding roller and the grinding groove body more easily, on the other hand, the graphite oxide fragments or the reflowing oxidized particles can be rolled and pushed to the periphery of the grinding gap, the graphite oxide fragments or the reflowing oxidized particles are dispersed, and the stacking is reduced, thereby avoiding the problem of plugging caused by accumulation; the left end of the second grinding roller is provided with the annular inclined plane, so that the graphite oxide fragments or the returned oxide particles falling from the upper side are drained and enter a grinding area.
As a further scheme of the invention, a scraping plate is fixedly connected to the inner side of the end part of the connecting frame corresponding to the position of the second grinding roller, the arc-shaped surface of the bottom of the scraping plate is contacted with the surface of the second grinding roller, a blade is fixedly connected to the side surface of the scraping plate, and the side surface of the blade is an arc-shaped surface; the during operation, at the in-process that rolls, the graphite oxide granule can be stained with on the surface of second grinding roller, influences the grinding quality, and through setting up the scraper blade, the scraper blade can be at the in-process that the second grinding roller ground, will grind the graphite oxide granule on roller surface and in time clear up to in the effect of blade, cutting power is stronger, and the clearance is more thorough, guarantees that the grinding quality of grinding roller next position obtains guaranteeing, can not receive to glue glutinous graphite oxide granule influence.
As a further scheme of the invention, the side surface of the scraper is fixedly connected with an arc-shaped cleaning block, and the inner wall of the arc-shaped cleaning block is contacted with the annular inclined surface at the end part of the second grinding roller; the during operation, carry out the in-process of drainage to the graphite oxide granule at the annular inclined plane of second grinding roller left end, the surface can glue and stick the graphite oxide granule, and drainage face frictional resistance increases, influences the drainage ability, through setting up arc clearance piece, can grind the rotatory in-process at the second grinding roller, and arc clearance piece is scraped relatively, clears up the graphite oxide granule on the annular inclined plane of grinding roller left end, guarantees the smoothness on grinding roller left end annular inclined plane, maintains stronger drainage ability.
As a further scheme of the invention, two sides of the inner wall of the U-shaped filter plate are fixedly connected with slide bars distributed in a linear array together, the surfaces of the slide bars are connected with two shunting plates with V-shaped cross sections in a sliding manner together, two sides of each shunting plate are provided with shunting ports distributed in a linear manner, and the right ends of the two shunting plates are connected with the U-shaped filter plate together through an elastic resetting mechanism; the during operation, when the oxidation graphite granule falls to U-shaped filter inside, it is comparatively concentrated, can't disperse on the U-shaped filter cross-section, influence the quality of filtering the screening, cause easily that the oxidation graphite granule that does not pass through the U-shaped filter but satisfies the granule needs to be discharged away, cause the repetition of processing, influence work efficiency, through setting up flow distribution plate and slide bar, the oxidation graphite granule that falls to in the U-shaped filter can be shunted by the space between flow distribution plate and the slide bar, the opening can be with partial oxidation graphite granule reposition of redundant personnel to the flow distribution plate inside with the filtration face of U-shaped filter dispersion of oxidation graphite granule, avoid causing piling up of oxidation graphite granule and cause the problem that the oxidation graphite granule that does not pass through the U-shaped filter but satisfies the granule needs to be discharged away, reduce repetitive processing, work efficiency has been improved indirectly.
As a further scheme of the invention, the elastic reset mechanism comprises two connecting sleeves, the two connecting sleeves are respectively and fixedly connected to the right sides of the two splitter plates, the inner walls of the two connecting sleeves are jointly and slidably connected with a supporting rod, two ends of the supporting rod are respectively and fixedly connected to the right side of the U-shaped filter plate through a first connecting plate, two ends of the surface of the supporting rod are respectively sleeved with a reset spring, and two ends of the reset spring are respectively and fixedly connected to the inner side of the first connecting plate and the side face of the connecting sleeve; the during operation, through setting up reset spring and bracing piece, played the position of shunting board and carried out elastic support, maintain the shunting position with the shunting board, and under the promotion of external force, can realize lateral sliding's effect, when losing the effort, carry out the function that in time resets, provide adjustable operating space for the shunting board, can manually stir two shunting boards to both sides, the oxidation graphite granule that will fall promotes to both sides, reach the area of diffusion oxidation graphite granule on the U-shaped filter filtering surface, obtain abundant filtration.
As a further scheme of the invention, the side surface of the connecting sleeve is fixedly connected with obliquely arranged driving plates, the two driving plates are distributed in a splayed manner, the surfaces of two supporting legs positioned on the right side are fixedly connected with a second connecting plate together, the positions of the top of the second connecting plate, which correspond to the end parts of the two driving plates, are rotatably connected with pushing columns, and the surfaces of the pushing columns are in mutual contact with the inner side inclined surfaces of the driving plates; the during operation, when the flow distribution plate shunts the graphite oxide granule, need manual stirring further the graphite oxide granule that the diffusion fell down, it is comparatively troublesome to operate, through setting up the drive plate, second connecting plate car and promotion post, in-process that the U-shaped filter was rocked by the linkage, can rock right, drive the drive plate and promote post interact, make the drive plate can drive the flow distribution plate and move to both sides certain extent, nevertheless can not break away from the reposition of redundant personnel region, when the U-shaped filter rocks left, the flow distribution plate can reset under reset spring's effect, the graphite oxide granule that will fall on the U-shaped filter filtering surface carries out the part to both sides and promotes, reach the effect that increases dispersion area, be favorable to abundant filtration, and need not manual operation, the operation is facilitated.
Compared with the prior art, the invention has the beneficial effects that:
1. according to the invention, the grinding motor, the grinding shaft, the first grinding roller, the grinding tank body, the fixing plate, the U-shaped filter plate, the collecting hopper, the T-shaped frame, the conveying pipe, the communicating pipe, the conveying motor, the conveying shaft, the conveying leaves, the collecting hopper, the driving gear, the follow-up fluted disc and the linkage rod are arranged, so that the grinding, screening and re-grinding work is automatically completed in one grinding device, the working processes are closely linked, separate operation is not needed, the time of manual transfer operation is saved, the working efficiency is improved, and the working progress of preparing graphene is ensured.
2. According to the invention, the second grinding roller is arranged, graphite oxide fragments or backflow oxidation particles on the inclined arc surface are rolled and rolled in advance, so that the fineness of the graphite oxide fragments or backflow oxidation particles is reduced, the graphite oxide fragments or backflow oxidation particles can more easily enter a grinding gap between the first grinding roller and the grinding groove body, and on the other hand, the graphite oxide fragments or backflow oxidation particles can be rolled and pushed to the periphery of the grinding gap to be dispersed, so that the accumulation is reduced, and the problem of blocking caused by accumulation is further avoided;
3. according to the invention, the ground graphite oxide particles can be shunted by arranging the sliding rod, the shunt plate, the supporting rod, the connecting sleeve, the return spring, the driving plate and the pushing column, so that the area of the diffusion graphite oxide particles on the filtering surface of the U-shaped filtering plate is reached, and the ground graphite oxide particles are fully filtered.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings used in the description of the embodiments will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art that other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a flow chart of a manufacturing process of the present invention;
FIG. 2 is a perspective view of the grinding apparatus of the present invention;
FIG. 3 is an enlarged view of a portion A;
FIG. 4 is a first perspective view of the polishing apparatus of the present invention, partially in section;
FIG. 5 is a second perspective view of the polishing apparatus of the present invention, partially in section;
FIG. 6 is a perspective view showing the connection between the splitter plate and the connecting sleeve according to the present invention;
fig. 7 is a perspective view, partially in section, showing the connection between the connection frame and the second polishing roll according to the present invention.
In the drawings, the components represented by the respective reference numerals are listed below:
grinding shell 1, grinding motor 2, grinding shaft 3, first grinding roller 4, grinding trough 5, fixing plate 6, supporting legs 7, base 8, U-shaped filter plate 9, collecting hopper 10, sliding block 11, sliding rail 12, T-shaped frame 13, conveying pipe 14, communicating pipe 15, conveying motor 16, conveying shaft 17, conveying blade 18, collecting hopper 19, driving gear 20, follow-up fluted disc 21, gangbar 22, connecting frame 23, second grinding roller 24, scraper 25, arc cleaning block 26, sliding rod 27, flow distribution plate 28, supporting rod 29, connecting sleeve 30, reset spring 31, driving plate 32 and pushing column 33.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Referring to fig. 1-7, the present invention provides a technical solution: a large-scale graphene preparation process comprises the following steps:
the method comprises the following steps: oxidizing graphite powder by concentrated sulfuric acid and potassium permanganate to prepare graphite oxide, and performing vacuum drying on the prepared graphite oxide;
step two: putting the graphite oxide after vacuum drying into grinding equipment for grinding, and then directly screening, wherein the graphite oxide is ground into particles of more than 300 meshes;
step three: putting the graphite oxide particles obtained by screening into a mixing container, adding ionized water according to the proportion that 300mg of graphite oxide particles are dispersed in 60ml of ionized water, and mixing by ultrasonic vibration to obtain colloidal suspension;
step four: then transferring the colloidal suspension into a stirring container, adding sodium borohydride and sodium dodecyl benzene sulfonate, heating to 80 ℃, refluxing for 16h under the condition, performing centrifugal separation, sequentially washing with acetone and deionized water until the pH value is 7, and performing vacuum drying on the obtained filter cake to obtain graphene;
wherein, the grinding device in the second step comprises a grinding shell 1, the two sides of the top of the grinding shell 1 are fixedly communicated with feed hoppers, the middle position of the top of the grinding shell 1 is fixedly connected with a grinding motor 2, the output end of the grinding motor 2 is fixedly connected with a grinding shaft 3, the bottom end of the grinding shaft 3 penetrates into the grinding shell 1 and is fixedly connected with a first grinding roller 4, a grinding groove body 5 which is matched and ground with the first grinding roller 4 is fixedly connected on the inner wall of the grinding shell 1, the top end of the inner wall of the grinding groove body 5 is provided with an inclined arc surface, the bottom of the grinding groove body 5 is fixedly connected with a discharge hopper, the lower surface of the grinding shell 1 is fixedly connected with a fixed plate 6, the four corners of the bottom of the fixed plate 6 are fixedly connected with supporting legs 7, the bottoms of the four supporting legs 7 are fixedly connected with a base 8 together, the top of the base 8, the backflow conveying mechanism shakes the grinding particle screening mechanism back and forth through the linkage mechanism;
the grinding particle screening mechanism comprises an obliquely arranged U-shaped filter plate 9, the lower end of the U-shaped filter plate 9 is fixedly connected with a backflow hopper, the bottom of the U-shaped filter plate 9 is fixedly connected with a collecting hopper 10 which is obliquely arranged in the opposite direction, two sides of the U-shaped filter plate 9 and the collecting hopper 10 are both fixedly connected with two supporting plates together, the bottoms of the two supporting plates on the same side are fixedly connected with a sliding block 11 together, the top of the base 8 is fixedly connected with a sliding rail 12 corresponding to the position of the sliding block 11, the sliding block 11 is connected onto the surface of the sliding rail 12 in a sliding mode, and a T-shaped;
the backflow conveying mechanism comprises a conveying pipe 14, the conveying pipe 14 is fixedly connected to the side face of the fixing plate 6, a communicating pipe 15 which is obliquely arranged is fixedly communicated with the top end of the side face of the conveying pipe 14, one end, far away from the conveying pipe 14, of the communicating pipe 15 is communicated with the top end of the side face of the grinding shell 1, a conveying motor 16 is fixedly connected to the top of the conveying pipe 14, a conveying shaft 17 is fixedly connected to the output end of the conveying motor 16, the bottom end of the conveying shaft 17 penetrates into the conveying pipe 14 and is fixedly connected with a conveying blade 18 on the surface of the conveying shaft, the bottom end of the conveying shaft 17 is rotatably connected to the top of the base 8, a material collecting hopper 19 is rotatably connected to the surface of the conveying shaft 17, a connecting seat is fixedly connected to the side face of the material collecting hopper 19 and is fixedly connected to the side face;
the linkage mechanism comprises a driving gear 20 and a follow-up gear disc 21, the driving gear 20 is fixedly connected to the surface of the conveying shaft 17 and is located at the position below the material collecting hopper 19, the follow-up gear disc 21 is rotatably connected to the top of the base 8, the follow-up gear is located between the driving gear 20 and the T-shaped frame 13, the side face of the follow-up gear is meshed with the side face of the driving gear 20, the left side of the top of the follow-up gear is fixedly connected with a first connecting shaft, the left end of the T-shaped frame 13 is fixedly connected with a second connecting shaft, and the second connecting shaft and the surface of the first;
during operation, the graphite oxide particles with unsatisfactory particle size exist in the fineness of the graphite oxide particles obtained by grinding the graphite oxide, a large amount of graphite oxide meeting the ideal fine mesh needs to be ground, so that a worker needs to grind the graphite oxide particles which are not satisfied with the single-time grinding again, then the graphite oxide particles are screened by a screening program, the whole operation process needs manual transfer and is troublesome, the working efficiency is too low, the preparation progress of the whole preparation process is influenced, the grinding, screening and re-grinding projects are completed on one device by arranging the first grinding roller 4, the grinding tank body 5, the grinding particle screening mechanism, the backflow conveying mechanism and the linkage mechanism, the grinding motor 2 and the conveying motor 16 are started by an external controller, and then the larger graphite oxide is thrown into the grinding shell 1 through the feed hopper after being broken, the grinding motor 2 drives the first grinding roller 4 to rotate through the grinding shaft 3, the first grinding roller 4 extrudes graphite oxide into a space between the first grinding roller 4 and the grinding groove body 5 for grinding, the ground graphite oxide particles are shunted to the inside of the U-shaped filter plate 9 through the discharge hopper for screening, the screening fine mesh of the U-shaped filter plate 9 is 300 meshes, meanwhile, the conveying motor 16 drives the conveying blade 18 and the driving gear 20 to rotate through the conveying shaft 17, the driving gear 20 drives the follow-up fluted disc 21 to rotate, the follow-up fluted disc 21 reciprocally links the T-shaped frame 13 through the linkage rod 22, the T-shaped frame 13 pulls the U-shaped filter plate 9 and the collecting hopper 10 to rock through the sliding block 11 and the supporting plate, the graphite oxide particles passing through the U-shaped filter plate 9 meet more than 300 meshes and meet the preparation requirement, are collected by the collecting hopper 10 and are drained out for direct use, meanwhile, the screened larger graphite oxide particles are drained to the inside the collecting hopper 10 through the backflow hopper, under the conveying action of the conveying blades 18, the large graphite oxide particles are vertically conveyed and flow back to the interior of the grinding shell 1 through the communicating pipe 15 for secondary grinding, manual operation is not needed in the whole process, grinding, screening and secondary grinding are automatically completed in one grinding device, the working process is closely linked, separate operation is not needed, the time of manual transfer operation is saved, the working efficiency is improved, and the working progress of preparing graphene is ensured; the inclined arc surface is formed at the top end of the inner wall of the grinding tank body 5, so that the introduced graphite oxide fragments or the returned oxidized particles are drained, and the graphite oxide fragments or the returned oxidized particles enter a gap between the first grinding roller 4 and the grinding tank body 5.
As a further scheme of the invention, the connecting frame 23 is fixedly connected to the surface of the grinding shaft 3 and positioned inside the grinding shell 1, the end part of the connecting frame 23 far away from the grinding shaft 3 is rotatably connected with a second grinding roller 24, the left end of the second grinding roller 24 is provided with an annular inclined plane, and the surface of the second grinding roller 24 is in contact with an inclined arc surface at the top of the inner wall of the grinding tank body 5; during operation, the graphite oxide fragments or the reflowing oxidized particles can not rapidly enter the grinding gap between the first grinding roller 4 and the grinding groove 5, can be stacked together and can not be dispersed, and can also cause overstock plugging to the inlet of the gap between the first grinding roller 4 and the grinding groove body 5, through arranging the second grinding roller 24, the grinding shaft 3 can drive the second grinding roller 24 to roll along the inclined arc surface at the top of the inner wall of the grinding groove body 5, the graphite oxide fragments or the reflowing oxidized particles on the inclined arc surface are rolled and rolled in advance, the fineness of the graphite oxide fragments or the reflowing oxidized particles is reduced, the graphite oxide fragments or the reflowing oxidized particles can more easily enter the grinding gap between the first grinding roller 4 and the grinding groove body 5, and on the other hand, the graphite oxide fragments or the reflowing oxidized particles can be rolled and pushed around the grinding gap, dispersing is carried out, so that accumulation is reduced, and the problem of plugging caused by accumulation is avoided; an annular inclined plane is formed at the left end of the second grinding roller 24, so that graphite oxide fragments or returned oxide particles falling from the upper side are drained and enter a grinding area.
As a further scheme of the invention, a scraper 25 is fixedly connected to the inner side of the end part of the connecting frame 23 corresponding to the position of the second grinding roller 24, the arc-shaped surface of the bottom of the scraper 25 is contacted with the surface of the second grinding roller 24, and a blade is fixedly connected to the side surface of the scraper 25, and the side surface of the blade is an arc-shaped surface; the during operation, at the in-process that rolls, the graphite oxide granule can be stained with on the surface of second grinding roller 24, influences the grinding quality, and through setting up scraper blade 25, scraper blade 25 can grind the in-process that roller 24 ground at the second, in time clears up the graphite oxide granule that grinds the roller surface to in the effect of blade, cutting power is stronger, clears up more thoroughly, guarantees that the grinding quality who grinds roller next position obtains guaranteeing, can not receive to glue glutinous graphite oxide granule influence.
As a further scheme of the invention, the side surface of the scraper 25 is fixedly connected with an arc-shaped cleaning block 26, and the inner wall of the arc-shaped cleaning block 26 is contacted with the annular inclined surface at the end part of the second grinding roller 24; the during operation, carry out the in-process of drainage to the graphite oxide granule at the annular inclined plane of 24 left ends of second grinding roller, the surface can glue and stick the graphite oxide granule, drainage face frictional resistance increases, influence drainage ability, through setting up arc clearance piece 26, can roll rotatory in-process at second grinding roller 24, arc clearance piece 26 is scraped relatively, will grind the graphite oxide granule on the annular inclined plane of roller left end and clear up, guarantee the smoothness of grinding roller left end annular inclined plane, maintain stronger drainage ability.
As a further scheme of the invention, two sides of the inner wall of the U-shaped filter plate 9 are fixedly connected with slide bars 27 distributed in a linear array together, the surfaces of the slide bars 27 are connected with two shunting plates 28 with V-shaped cross sections together in a sliding manner, two sides of each shunting plate 28 are provided with shunting ports distributed in a linear manner, and the right ends of the two shunting plates 28 are connected with the U-shaped filter plate 9 together through an elastic resetting mechanism; when the device works, when graphite oxide particles fall into the U-shaped filter plate 9, the graphite oxide particles are concentrated and can not be dispersed on the filtering surface of the U-shaped filter plate 9, the filtering and screening quality is influenced, the graphite oxide particles which do not pass through the U-shaped filter plate 9 but meet the particle requirements are easily discharged, the processing is repeated, and the working efficiency is influenced, through setting up flow distribution plate 28 and slide bar 27, the graphite oxide granule that falls to in the U-shaped filter 9 can be shunted by the space between flow distribution plate 28 and the slide bar 27, the opening can shunt partial graphite oxide granule to the inside filtering surface with the graphite oxide granule dispersion to U-shaped filter 9 of flow distribution plate 28, avoid causing piling up of graphite oxide granule and cause the problem that the graphite oxide granule that does not satisfy the granule needs through U-shaped filter 9 is arranged away, reduce repetitive processing, the indirect work efficiency that has improved.
As a further scheme of the invention, the elastic reset mechanism comprises two connecting sleeves 30, the two connecting sleeves 30 are respectively fixedly connected to the right sides of the two splitter plates 28, the inner walls of the two connecting sleeves 30 are jointly and slidably connected with a supporting rod 29, both ends of the supporting rod 29 are fixedly connected to the right side of the U-shaped filter plate 9 through a first connecting plate, both ends of the surface of the supporting rod 29 are respectively sleeved with a reset spring 31, and both ends of the reset spring 31 are respectively and fixedly connected to the inner side of the first connecting plate and the side surface of the connecting sleeve 30; the during operation, through setting up reset spring 31 and bracing piece 29, played and carried out elastic support to the position of flow distribution plate 28, maintain flow distribution plate 28 at the reposition of redundant personnel position, and under the promotion of external force, can realize lateral sliding's effect, when losing the effort, the function that in time resets carries out, provide adjustable operating space for flow distribution plate 28, can manually stir two flow distribution plates to both sides, the oxidation graphite granule that will fall promotes to both sides, reach the area of diffusion oxidation graphite granule on U-shaped filter 9 cross filter face, obtain abundant filtration.
As a further scheme of the invention, the side surface of the connecting sleeve 30 is fixedly connected with driving plates 32 which are obliquely arranged, the two driving plates 32 are distributed in a splayed shape, the surfaces of the two supporting legs 7 positioned at the right side are fixedly connected with a second connecting plate together, the positions of the top of the second connecting plate, which correspond to the end parts of the two driving plates 32, are both rotatably connected with pushing columns 33, and the surfaces of the pushing columns 33 are mutually contacted with the inner inclined surfaces of the driving plates 32; the during operation, when flow distribution plate 28 shunts the graphite oxide granule, need manual stirring further the graphite oxide granule that the diffusion fell down, it is comparatively troublesome to operate, through setting up drive plate 32, second connecting plate car and promotion post 33, in-process that U-shaped filter 9 was rocked by the linkage, can rock right, drive plate 32 and promote post 33 interact, make drive plate 32 can drive flow distribution plate 28 and remove to both sides certain range, nevertheless can not break away from the reposition of redundant personnel region, when U-shaped filter 9 rocks left, flow distribution plate 28 can reset under reset spring 31's effect, the graphite oxide granule that will fall to on the U-shaped filter 9 filtering surface carries out the part to both sides and promotes, reach the effect that increases the dispersed area, be favorable to the abundant filtration, and need not manual operation, the operation is made things convenient for the operation.
The working principle is as follows: during operation, the graphite oxide particles with unsatisfactory particle size exist in the fineness of the graphite oxide particles obtained by grinding the graphite oxide, a large amount of graphite oxide meeting the ideal fine mesh needs to be ground, so that a worker needs to grind the graphite oxide particles which are not satisfied with the single-time grinding again, then the graphite oxide particles are screened by a screening program, the whole operation process needs manual transfer and is troublesome, the working efficiency is too low, the preparation progress of the whole preparation process is influenced, the grinding, screening and re-grinding projects are completed on one device by arranging the first grinding roller 4, the grinding tank body 5, the grinding particle screening mechanism, the backflow conveying mechanism and the linkage mechanism, the grinding motor 2 and the conveying motor 16 are started by an external controller, and then the larger graphite oxide is thrown into the grinding shell 1 through the feed hopper after being broken, the grinding motor 2 drives the first grinding roller 4 to rotate through the grinding shaft 3, the first grinding roller 4 extrudes graphite oxide into a space between the first grinding roller 4 and the grinding groove body 5 for grinding, the ground graphite oxide particles are shunted to the inside of the U-shaped filter plate 9 through the discharge hopper for screening, the screening fine mesh of the U-shaped filter plate 9 is 300 meshes, meanwhile, the conveying motor 16 drives the conveying blade 18 and the driving gear 20 to rotate through the conveying shaft 17, the driving gear 20 drives the follow-up fluted disc 21 to rotate, the follow-up fluted disc 21 reciprocally links the T-shaped frame 13 through the linkage rod 22, the T-shaped frame 13 pulls the U-shaped filter plate 9 and the collecting hopper 10 to rock through the sliding block 11 and the supporting plate, the graphite oxide particles passing through the U-shaped filter plate 9 meet more than 300 meshes and meet the preparation requirement, are collected by the collecting hopper 10 and are drained out for direct use, meanwhile, the screened larger graphite oxide particles are drained to the inside the collecting hopper 10 through the backflow hopper, under the conveying action of the conveying blades 18, the large graphite oxide particles are vertically conveyed and flow back to the interior of the grinding shell 1 through the communicating pipe 15 for secondary grinding, manual operation is not needed in the whole process, grinding, screening and secondary grinding are automatically completed in one grinding device, the working process is closely linked, separate operation is not needed, the time of manual transfer operation is saved, the working efficiency is improved, and the working progress of preparing graphene is ensured; the inclined arc surface is formed at the top end of the inner wall of the grinding tank body 5, so that the introduced graphite oxide fragments or the returned oxidized particles are drained, and the graphite oxide fragments or the returned oxidized particles enter a gap between the first grinding roller 4 and the grinding tank body 5.
In the description herein, references to the description of "one embodiment," "an example," "a specific example" or the like are intended to mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The preferred embodiments of the invention disclosed above are intended to be illustrative only. The preferred embodiments are not intended to be exhaustive or to limit the invention to the precise embodiments disclosed. Obviously, many modifications and variations are possible in light of the above teaching. The embodiments were chosen and described in order to best explain the principles of the invention and the practical application, to thereby enable others skilled in the art to best utilize the invention. The invention is limited only by the claims and their full scope and equivalents.
Claims (7)
1. A large-scale graphene preparation process is characterized by comprising the following steps: the process comprises the following steps:
the method comprises the following steps: oxidizing graphite powder by concentrated sulfuric acid and potassium permanganate to prepare graphite oxide, and performing vacuum drying on the prepared graphite oxide;
step two: putting the graphite oxide after vacuum drying into grinding equipment for grinding, and then directly screening, wherein the graphite oxide is ground into particles of more than 300 meshes;
step three: putting the graphite oxide particles obtained by screening into a mixing container, adding ionized water according to the proportion that 300mg of graphite oxide particles are dispersed in 60ml of ionized water, and mixing by ultrasonic vibration to obtain colloidal suspension;
step four: then transferring the colloidal suspension into a stirring container, adding sodium borohydride and sodium dodecyl benzene sulfonate, heating to 80 ℃, refluxing for 16h under the condition, performing centrifugal separation, sequentially washing with acetone and deionized water until the pH value is 7, and performing vacuum drying on the obtained filter cake to obtain graphene;
wherein, in the second step, the grinding device comprises a grinding shell (1), the two sides of the top of the grinding shell (1) are fixedly communicated with feed hoppers, the middle position of the top of the grinding shell (1) is fixedly connected with a grinding motor (2), the output end of the grinding motor (2) is fixedly connected with a grinding shaft (3), the bottom end of the grinding shaft (3) penetrates into the grinding shell (1) and is fixedly connected with a first grinding roller (4), the inner wall of the grinding shell (1) is fixedly connected with a grinding groove body (5) which is matched and ground with the first grinding roller (4), the top end of the inner wall of the grinding groove body (5) is provided with an inclined arc surface, the bottom of the grinding groove body (5) is fixedly connected with a discharge hopper, the lower surface of the grinding shell (1) is fixedly connected with a fixed plate (6), and four corners of the bottom of the fixed plate (6) are, the bottoms of the four supporting legs (7) are fixedly connected with a base (8) together, the top of the base (8) is connected with a grinding particle screening mechanism in a sliding mode, the side face of the fixed plate (6) is connected with a backflow conveying mechanism for enabling grinding particles to flow back into the grinding shell (1), and the backflow conveying mechanism shakes the grinding particle screening mechanism back and forth through a linkage mechanism;
the grinding particle screening mechanism comprises an obliquely arranged U-shaped filter plate (9), the lower end of the U-shaped filter plate (9) is fixedly connected with a return hopper, the bottom of the U-shaped filter plate (9) is fixedly connected with a collection hopper (10) which is obliquely arranged in the opposite direction, two sides of the U-shaped filter plate (9) and the collection hopper (10) are both fixedly connected with two support plates together, the bottoms of the two support plates on the same side are fixedly connected with a sliding block (11) together, the top of the base (8) is fixedly connected with a sliding rail (12) corresponding to the position of the sliding block (11), the sliding block (11) is connected on the surface of the sliding rail (12) in a sliding mode, and a T-shaped frame (13) is fixedly connected;
the backflow conveying mechanism comprises a conveying pipe (14), the conveying pipe (14) is fixedly connected to the side face of a fixing plate (6), a communicating pipe (15) which is obliquely arranged is fixedly communicated with the top end of the side face of the conveying pipe (14), one end, far away from the conveying pipe (14), of the communicating pipe (15) is communicated with the top end of the side face of a grinding shell (1), a conveying motor (16) is fixedly connected to the top of the conveying pipe (14), a conveying shaft (17) is fixedly connected to the output end of the conveying motor (16), the bottom end of the conveying shaft (17) penetrates into the conveying pipe (14) and is fixedly connected to conveying leaves (18) on the surface of the conveying shaft, the bottom end of the conveying shaft (17) is rotatably connected to the top of a base (8), a collecting hopper (19) is rotatably connected to the surface of the conveying shaft (17), and a, the connecting seat is fixedly connected to the side face of the base (8), the bottom end of the conveying pipe (14) is positioned in the collecting hopper (19) and close to the bottom of the inner wall of the collecting hopper (19), and the end part of the discharging hopper extends to the position, close to the conveying pipe (14), of the top of the collecting hopper (19);
the link gear includes drive gear (20) and follow-up fluted disc (21), drive gear (20) fixed connection is in carrying axle (17) position that just is located collecting hopper (19) below on the surface, follow-up fluted disc (21) rotate to be connected at base (8) top to the follow-up gear is located between drive gear (20) and T shape frame (13), follow-up gear side and drive gear (20) side intermeshing, follow-up gear top left side fixedly connected with first connecting axle, T shape frame (13) left end fixedly connected with second connecting axle, the common rotation on the surface of second connecting axle and first connecting axle is connected with gangbar (22).
2. The large-scale graphene preparation process according to claim 1, which is characterized in that: grind axle (3) surface and be located the inside fixedly connected with link (23) of grinding casing (1), the tip that the axle (3) was kept away from in link (23) rotates and is connected with second grinding roller (24), annular inclined plane has been seted up to the left end that second grinding roller (24), the surface that second grinding roller (24) and the slope arc surface at grinding groove body (5) inner wall top contact each other.
3. The large-scale graphene preparation process according to claim 2, which is characterized in that: the inboard second that corresponds of link (23) tip grinds roller (24) position fixedly connected with scraper blade (25), scraper blade (25) bottom arcwall face and second grind roller (24) surface and contact each other, and the side fixedly connected with blade of scraper blade (25), the blade side is the arcwall face.
4. The large-scale graphene preparation process according to claim 3, which is characterized in that: the side fixedly connected with arc clearance piece (26) of scraper blade (25), the inner wall of arc clearance piece (26) and the annular inclined plane of second grinding roller (24) tip contact each other.
5. The large-scale graphene preparation process according to claim 1, which is characterized in that: the U-shaped filter plate structure is characterized in that two sides of the inner wall of the U-shaped filter plate (9) are fixedly connected with slide rods (27) distributed in a linear array mode, the slide rods (27) are connected with two flow distribution plates (28) with V-shaped cross sections in a sliding mode on the surface, flow distribution ports distributed in a linear mode are formed in the two sides of each flow distribution plate (28), and the right ends of the flow distribution plates (28) are connected with the U-shaped filter plate (9) through elastic reset mechanisms.
6. The large-scale graphene preparation process according to claim 5, which is characterized in that: elasticity canceling release mechanical system includes two adapter sleeves (30), two adapter sleeve (30) fixed connection respectively is on the right side of two flow distribution plates (28), and the common sliding connection of inner wall of two adapter sleeves (30) has bracing piece (29), the both ends of bracing piece (29) all are on U-shaped filter (9) right side through first connecting plate fixed connection, reset spring (31) have all been cup jointed at the both ends on bracing piece (29) surface, the both ends difference fixed connection of reset spring (31) is inboard and adapter sleeve (30) side at first connecting plate.
7. The large-scale graphene preparation process according to claim 6, which is characterized in that: drive plate (32) that the side fixedly connected with slope of adapter sleeve (30) set up, two drive plate (32) are the splayed subsection, are located two supporting legs (7) on right side common fixedly connected with second connecting plate in surface, the equal rotation in position that corresponds two drive plate (32) tip in second connecting plate top is connected with promotion post (33), promote post (33) surface and drive plate (32) inboard inclined plane and contact each other.
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| CN202010459451.7A CN111620328A (en) | 2020-05-27 | 2020-05-27 | Large-scale graphene preparation process |
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