CN109835889B - Mechanical stripping device for graphene and graphene preparation method - Google Patents
Mechanical stripping device for graphene and graphene preparation method Download PDFInfo
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- CN109835889B CN109835889B CN201910303579.1A CN201910303579A CN109835889B CN 109835889 B CN109835889 B CN 109835889B CN 201910303579 A CN201910303579 A CN 201910303579A CN 109835889 B CN109835889 B CN 109835889B
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Abstract
The invention discloses a mechanical stripping device for graphene, which comprises a stripping tank body, wherein a feeding hole and a discharging hole are formed in the stripping tank body; an inner chamber at one end of the stripping tank body is a feeding chamber, an inner chamber at the other end of the stripping tank body is a discharging chamber, the feeding chamber and the discharging chamber are provided with a rectifying section and a shearing stripping section positioned on the discharging side of the rectifying section, a material return pipeline is communicated between the discharging chamber and the feeding chamber, and a feeding pump is arranged on the material return pipeline; the rectifying section comprises a plurality of clapboards, the side edges of the clapboards are connected with a stripping tank body, the inner chamber of the rectifying section is separated into a plurality of flat gaps by the clapboards, the gaps are consistent with the axial direction of the stripping tank body, a plurality of fixed knives are arranged in the shearing stripping section, a discharge channel is arranged between the fixed knives, the two ends of the fixed knives are connected with the stripping tank body, and the cutting edges of the fixed knives face the discharge end of the rectifying section. The mechanical graphene stripping device is provided with a gap, so that the graphite is fixed and oriented in a gap fluid, the impact of the non-orthogonal force of the side surface of the graphene lamination and the blade part is increased, and effective stripping is realized.
Description
Technical Field
The invention relates to the technical field of graphene stripping machinery, in particular to a mechanical graphene stripping device and a graphene preparation method.
Background
The production method of graphene mainly comprises a mechanical stripping method, a chemical deposition method, a reduced graphene oxide method and a direct solvent stripping method according to the principle. The mechanical stripping method and the chemical vapor deposition method can obtain graphene with high aspect ratio, but the yield is low compared with the chemical vapor deposition method. The reduced graphene oxide method can realize low-cost large-scale preparation of graphene, but the obtained graphene contains a large number of defects, and solvent stripping methods such as N-methylpyrrolidone (NMP) and N, N-Dimethylformamide (DMF) generally have the defects of toxicity and high boiling point. The solvent stripping method generally combines auxiliary means such as ultrasound, heat treatment, microwave irradiation and the like to increase the gaps between graphene layers. In the mechanical stripping equipment in the prior art, for example, CN106865530A, CN104370283A, and CN104477882A, the stripping equipment in the three steps disperses flake graphite or expanded graphite in a fluid, and drives the fluid to move by using a stirring member, so that the fluid and fixed teeth or movable teeth in a container collide relatively to each other, a shearing force is applied to the graphite, and finally, the synergy of graphene mechanical stripping is realized. However, the fluid movement modes in the three schemes are turbulent flows or eddy flows, and the arrangement direction of graphene in the fluid is disordered, that is, the fixed teeth or the movable teeth collide with graphite, for example, by ball milling, so that the size of the graphene is smaller, and the diameter-thickness ratio of the graphene is lower.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provide a mechanical graphene stripping device, so that graphene forms fixed orientation in a gap, the probability of collision between a blade and the side face of a graphene lamination is increased, and the size and the radius-thickness ratio of the graphene are improved.
In order to achieve the technical effects, the technical scheme of the invention is as follows: the mechanical stripping device for graphene is characterized by comprising a stripping tank body, wherein a feeding hole and a discharging hole are formed in the stripping tank body; an inner chamber at one end of the stripping tank body is a feeding chamber, an inner chamber at the other end of the stripping tank body is a discharging chamber, the feeding chamber and the discharging chamber are provided with a rectifying section and a shearing stripping section positioned on the discharging side of the rectifying section, a material return pipeline is communicated between the discharging chamber and the feeding chamber, and a feeding pump is arranged on the material return pipeline;
the rectifying section comprises a plurality of clapboards, the side edges of the clapboards are connected with the stripping tank body, the inner chamber of the rectifying section is separated into a plurality of flat gaps by the clapboards, the gaps are consistent with the axial direction of the stripping tank body, a plurality of fixed knives are arranged in the shearing stripping section, a discharge channel is arranged between the fixed knives, the two ends of the fixed knives are connected with the stripping tank body, and the cutting edges of the fixed knives face the discharge end of the rectifying section.
The preferable technical scheme is that the peeling device further comprises a heating element, and the heating element is arranged outside the peeling tank body and/or in the partition plate.
The preferable technical scheme is that the distance between adjacent partition plates is gradually reduced from the feeding end to the discharging end of the rectifying section.
The preferred technical scheme is that the baffle is provided with a flow guide strip, a gap exists between the flow guide strip and the adjacent baffle, and the flow guide strip is consistent with the axial direction of the stripping tank body.
The preferred technical scheme is that the feeding end face of the flow guide strip is flush with the partition plate, the interval of the adjacent partition plates, the length of the flow guide strip along the axial direction of the stripping tank body and the length of the partition plate are in a ratio of (0.1-0.5): (3-4): 6.
The preferred technical scheme is that the ratio of the gap feeding end surface and the gap discharging end surface formed by enclosing the partition plate and the stripping tank body is 5: (1-2).
The preferable technical scheme is that an ultrasonic vibration plate is arranged in the feeding chamber and/or the discharging chamber and is connected with an ultrasonic generator outside the stripping tank body.
The optimized technical scheme is that the cross section of the fixed knife is in an airfoil shape, the first knife face of the fixed knife is a folding face with a folding angle in smooth transition, the second knife face is a plane or a smooth arc face, the first knife face and the second knife face are intersected at a knife edge and a knife back, the knife edge and the knife back are both in a sharp edge shape, the protrusion height of the first knife face is higher than that of the second knife face, and the first knife faces of two adjacent fixed knives are arranged adjacently.
The invention also aims to provide a graphene preparation method, which is characterized by comprising the following mechanical stripping steps: dispersing crystalline flake graphite or expanded graphite in a solvent to form a graphene suspension, introducing the graphene suspension into a stripping tank body, starting a feed pump, and circulating the suspension in a closed passage formed by the stripping tank body and a return pipeline.
The preferable technical scheme is that the method further comprises the following ultrasonic treatment steps: starting an ultrasonic generator, and ultrasonically treating the graphene suspension in the stripping tank body; the ultrasonic treatment step and the mechanical peeling step are alternately carried out.
The invention has the advantages and beneficial effects that:
gaps are arranged in a stripping tank body in the mechanical stripping device for graphene, graphite forms fixed orientation in gap fluid by utilizing the characteristic that fluid flows in the gaps are distributed, impact of non-orthogonal force between the side surface of a graphene lamination and a blade part is increased, impact of orthogonal force between crystalline flake graphite and an expanded graphite sheet in the stripping process is reduced and controlled, and stripping probability caused by sliding between graphene layers is improved;
compared with mechanical stripping such as vortex, turbulence and the like in the prior art, the average size and the radius-thickness ratio of the graphene obtained by the method are improved;
the stationary knife is fixedly connected with the stripping tank body, the structure is stable, the flow rate of fluid is adjusted through the feeding pump, and the service life of the mechanical stripping equipment is long.
Drawings
Fig. 1 is a schematic structural view of a mechanical graphene exfoliation apparatus according to example 1;
FIG. 2 is an enlarged view of a portion of FIG. 1;
fig. 3 is a schematic structural view of a mechanical graphene peeling apparatus according to example 2;
FIG. 4 is a schematic structural view of a separator in example 3;
FIG. 5 is a graph showing the change in the flow direction of the fluid around the fixed blade in example 4.
In the figure: 1. stripping the tank body; 11. a feed chamber; 12. a discharge chamber; 13. a rectifying section; 14. a shear stripping section; 2. a feed inlet; 3. a discharge port; 4. fixing a cutter; 41. A first blade face; 42. a second blade surface; 43. a blade; 44. a back of a knife; 5. a feed back pipeline; 6. a feed pump; 7. a partition plate; 8. an ultrasonic vibration plate; 9. an ultrasonic generator; 10. a flow guide strip; a. a gap.
Detailed Description
The following description of the embodiments of the present invention will be made with reference to the accompanying drawings. The following examples are only for illustrating the technical solutions of the present invention more clearly, and the protection scope of the present invention is not limited thereby.
Feed pump
The specific type of the charge pump is not particularly limited, and further, in order to avoid random collision between the charge pump with the impeller and the graphene, the charge pump is a pump body without the impeller, and the selection range includes a reciprocating pump or a rotor pump.
Rectifying section
The effect of the flow straightening section is to guide the flow in a laminar manner, and the flow velocity of the flow in the flow straightening section is increased in the cross section of the flow straightening section compared with that in the feed chamber due to the presence of the partition. The size of the gap is specifically determined according to the viscosity, flow rate, and the like of the fluid. In order to avoid the mutual influence of the fluid between the gaps, the preferable technical proposal is that the side edge of the clapboard is connected with the stripping tank body in a sealing way.
Shear stripping section
The shearing and stripping section has the effects that the blade is utilized to shear the oriented graphite sheet layer, the thickness of the blade of the fixed cutter is controlled to be smaller, the theoretical thickness of the single-layer graphene is about 0.34nm, the thickness measured in an actual test is slightly larger than the theoretical thickness and is about 0.4-0.7 nm, therefore, the preferable fixed cutter is a diamond cutter, and the radius of the blade of the diamond cutter is selected to be smaller. The fixed cutter is arranged densely, and the stripping speed is accelerated.
Because the fluid of the ejection of compact of section of rectifying is laminar flow motion, consequently cut the stationary knife of peeling off the section and can set up one row that parallels or is similar to parallel with the section discharge gate of rectifying, also can set up the multirow, the stationary knife dislocation set of adjacent row satisfies the cutting edge towards the discharge end of rectifying section, and is specific, the stationary knife cutting edge that is close to the rectifying section is towards the discharge end in gap.
The stripping tank body can also be provided with a plurality of rectifying sections and shearing stripping sections which are arranged at intervals.
Heating element
The heating element serves to heat the fluid, and its structure and type are not particularly limited. Specifically, the stripping tank body is a jacket type tank body. Under the condition of no heating, the fluid also has small temperature rise due to the friction force between the fluid and the stripping tank body, the partition plate, the fixed knife, the return pipeline and the feeding pump in the long-time fluid circulation process. Therefore, in order to ensure that the temperature of the fluid is in a proper range, the return pipeline is also connected with a heat exchange cooling device.
Spacing of adjacent partitions
The distance between the adjacent partition plates is gradually reduced from the feeding end to the discharging end of the rectifying section, so that the fluid can be sprayed out of the rectifying section in a laminar flow jet shape, the flow velocity of the fluid is increased, and the graphite impact interaction force is increased.
Wing-shaped fixed cutter
The flow velocity of the fluid outside the first knife face of the wing-shaped fixed knife is higher, and the flow velocity of the fluid outside the second knife face is lower, so that the structure is beneficial to further optimizing the effects that the graphene layer is stressed to slide and is stripped. The row number of the multiple rows of fixed cutters is specifically determined according to the distribution condition of laminar flow of the fluid after the fixed cutters, and is usually 2-5 rows.
Mechanical stripping off device of graphite alkene
The expanded graphite is intercalated by the intercalation agent, so that the distance between graphene sheets is increased, and compared with flake graphite, the expanded graphite is more beneficial to obtaining graphene with larger size.
Example 1
As shown in fig. 1-2, the mechanical graphene stripping device in embodiment 1 includes a stripping tank 1, where the stripping tank 1 is provided with a feed inlet 2 and a discharge outlet 3; an inner chamber at one end of the stripping tank body 1 is a feeding chamber 11, an inner chamber at the other end of the stripping tank body is a discharging chamber 12, the feeding chamber 11 and the discharging chamber 12 are provided with a rectifying section 13 and a shearing stripping section 14 positioned on the discharging side of the rectifying section 13, a return pipeline 5 is communicated between the discharging chamber 12 and the feeding chamber 11, and a feeding pump 6 is arranged on the return pipeline 5;
the rectifying section 13 comprises a plurality of partition plates 7, the side edges of the partition plates 7 are connected with the stripping tank body 1, the partition plates 7 divide an inner chamber of the rectifying section 13 into a plurality of flat gaps a, the gaps a are consistent with the axial direction of the stripping tank body 1, a plurality of fixed knives 4 are arranged in the shearing stripping section 14, intervals are arranged among the fixed knives 4 and are discharging channels, the two ends of the fixed knives 4 are connected with the stripping tank body 1, and the cutting edges of the fixed knives 4 face the discharging end of the rectifying section 13.
The stripped can of example 1 was a jacket heated can. As an equivalent alternative, the heating element is disposed within the barrier, or both the exterior of the peel pot and the barrier.
Example 2
As shown in fig. 3, embodiment 2 differs from embodiment 1 in that the distance between adjacent baffle plates 7 gradually decreases from the feed end to the discharge end of the rectifying section 13.
In addition, in the embodiment 2, the feeding chamber 11 and the discharging chamber 12 are both provided with the ultrasonic vibration plate 8, and the ultrasonic vibration plate 8 is connected with the ultrasonic generator 9 outside the stripping tank body 1.
Example 3
As shown in fig. 4, embodiment 3 is based on embodiment 2, and is different in that a baffle 7 is provided with a flow guide strip 10, a gap exists between the flow guide strip 10 and an adjacent baffle, and the flow guide strip 10 is axially consistent with the peeled can body 1.
The feeding end face of the flow guide strip 10 is flush with the partition plates 7, the interval of the adjacent partition plates 7, the ratio of the length of the flow guide strip along the axial direction of the stripping tank body 1 to the length of the partition plates 7 is (0.05-0.2): (3-4): 6.
The ratio of the feeding end face to the discharging end face of the gap formed by the partition board 7 and the stripping tank body 1 in a surrounding manner is 5: (1-2).
Example 4
As shown in fig. 5, the embodiment 4 is based on the embodiment 3, and is different in that the cross section of the fixed blade 4 is an airfoil shape, the first blade surface 41 of the fixed blade 4 is a folded surface with a smoothly-transitioned folded corner, the second blade surface 42 is a smooth arc surface, the first blade surface 41 and the second blade surface 42 intersect at the blade edge 43 and the blade back 44, the blade edge 43 and the blade back 44 are both sharp-edged, and the protrusion height of the first blade surface 41 is higher than that of the second blade surface 42.
Further, in the embodiment 4, two adjacent fixed knives 4 are a fixed knife group, and the first knife faces 41 of the two fixed knives in the fixed knife group are arranged adjacently.
The graphene preparation method comprises the following mechanical stripping steps: dispersing crystalline flake graphite or expanded graphite in a solvent to form a graphene suspension, introducing the graphene suspension into a stripping tank body, starting a heating element to heat a dispersion liquid to 80-150 ℃, starting a feed pump, circularly treating the suspension in a closed passage formed by the stripping tank body and a return pipeline, standing, centrifuging, taking supernatant liquid, carrying out vacuum filtration, washing a filter cake with ethanol, transferring the filter cake into a freeze dryer, and carrying out freeze drying to obtain a graphene product.
The graphene preparation method further comprises the ultrasonic treatment step of: starting an ultrasonic generator, and ultrasonically treating the graphene suspension in the stripping tank body; the ultrasonic treatment step and the mechanical peeling step are alternately carried out. The ultrasonic treatment step and the mechanical stripping step are alternately treated, so that the yield of the graphene can be improved.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the technical principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (6)
1. The mechanical stripping device for graphene is characterized by comprising a stripping tank body, wherein a feeding hole and a discharging hole are formed in the stripping tank body; an inner chamber at one end of the stripping tank body is a feeding chamber, an inner chamber at the other end of the stripping tank body is a discharging chamber, the feeding chamber and the discharging chamber are provided with a rectifying section and a shearing stripping section positioned on the discharging side of the rectifying section, a material return pipeline is communicated between the discharging chamber and the feeding chamber, and a feeding pump is arranged on the material return pipeline;
the rectifying section comprises a plurality of partition plates, the side edges of the partition plates are connected with the stripping tank body, an inner chamber of the rectifying section is divided into a plurality of flat gaps by the partition plates, the gaps are consistent with the axial direction of the stripping tank body, a plurality of fixed knives are arranged in the shearing stripping section, a discharge channel is arranged between the fixed knives, two ends of each fixed knife are connected with the stripping tank body, and the cutting edges of the fixed knives face the discharge end of the rectifying section;
the distance between every two adjacent partition plates is gradually reduced from the feeding end to the discharging end of the rectifying section;
the cross section of the fixed cutter is in an airfoil shape, the first cutter face of the fixed cutter is a folding face with a folding angle in smooth transition, the second cutter face is a plane or a smooth arc face, the first cutter face and the second cutter face are intersected at a cutter edge and a cutter back, the cutter edge and the cutter back are both in a sharp edge shape, and the protrusion height of the first cutter face is higher than that of the second cutter face.
2. The mechanical graphene stripping apparatus according to claim 1, further comprising a heating element disposed outside the stripping can and/or within the separator.
3. The graphene mechanical stripping device according to claim 1, wherein a baffle plate is provided with a flow guide strip, a gap exists between the flow guide strip and an adjacent baffle plate, and the flow guide strip is in axial alignment with the stripping tank body.
4. The graphene mechanical stripping device according to claim 3, wherein the feeding end face of each flow guide strip is flush with the partition plate, and the ratio of the length of each flow guide strip to the length of each partition plate along the axial direction of the stripping tank at the interval between adjacent partition plates is (0.05-0.2): (3-4): 6.
5. The graphene mechanical stripping device according to claim 1, wherein the ratio of the feeding end face to the discharging end face of the gap formed by the partition board and the stripping tank body is 5: (1-2).
6. The graphene mechanical stripping device according to claim 1, wherein an ultrasonic vibration plate is arranged in the feeding chamber and/or the discharging chamber, and the ultrasonic vibration plate is connected with an ultrasonic generator outside the stripping tank body.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201910303579.1A CN109835889B (en) | 2019-04-16 | 2019-04-16 | Mechanical stripping device for graphene and graphene preparation method |
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| CN201910303579.1A CN109835889B (en) | 2019-04-16 | 2019-04-16 | Mechanical stripping device for graphene and graphene preparation method |
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| CN109835889B true CN109835889B (en) | 2022-02-18 |
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Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110282618B (en) * | 2019-07-23 | 2022-09-23 | 无锡乘臻科技有限公司 | Large-scale graphite alkene ultrasonic stripping off device |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104477882B (en) * | 2014-10-23 | 2016-06-29 | 江阴碳谷科技有限公司 | A kind of eddy current type Graphene stripping off device, Graphene production system and production method |
| CN105363535A (en) * | 2015-09-10 | 2016-03-02 | 江阴碳谷科技有限公司 | Dry graphene stripping device, production system and method for producing dry graphene |
| CA2972284C (en) * | 2016-07-05 | 2019-05-14 | Vln Advanced Technologies Inc. | Apparatus and method for preparing graphene by exfoliation of graphite using a pulsed or cavitating waterjet |
| CN106564888A (en) * | 2016-10-26 | 2017-04-19 | 成都新柯力化工科技有限公司 | Method of preparing graphene nanoplate size through nanometer-distribution collision stripping and graphene nanoplate size |
| CN106744871B (en) * | 2016-11-11 | 2018-09-18 | 新奥科技发展有限公司 | The pretreatment unit and method of graphite raw material, graphitized mesophase body and graphene |
| CN106927456A (en) * | 2017-04-05 | 2017-07-07 | 无锡泰科纳米新材料有限公司 | A kind of use mechanical stripping method prepares the process units and method of Graphene |
| CN206767653U (en) * | 2017-04-13 | 2017-12-19 | 成都新柯力化工科技有限公司 | A kind of flow-guiding type extruder that graphene is prepared for continuous stripping |
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