CN112125300A - Device and method for industrially and continuously preparing graphene slurry - Google Patents
Device and method for industrially and continuously preparing graphene slurry Download PDFInfo
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- CN112125300A CN112125300A CN201910554515.9A CN201910554515A CN112125300A CN 112125300 A CN112125300 A CN 112125300A CN 201910554515 A CN201910554515 A CN 201910554515A CN 112125300 A CN112125300 A CN 112125300A
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Classifications
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/184—Preparation
- C01B32/19—Preparation by exfoliation
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2204/00—Structure or properties of graphene
- C01B2204/20—Graphene characterized by its properties
- C01B2204/22—Electronic properties
Abstract
The invention relates to a device and a method for industrially and continuously preparing graphene slurry. The preparation device comprises a liquid nitrogen roller press instrument, a stirring kettle, an ultrasonic pipeline, a liquid storage tank and a bubble removing instrument. Grinding the mixture of the graphite-containing material and the liquid nitrogen by a liquid nitrogen roller mill by means of embrittlement and intercalation of the liquid nitrogen to obtain a pre-grinding material; transferring to a stirring kettle, adding materials containing solvent and the like under stirring to obtain uniform mixed materials; further stripping, cracking and compactly combining the components of the graphene mixed material in the S-shaped pipeline by adopting an ultrasonic dispersion technology; and buffering the dispersion liquid by a liquid storage tank, and performing centrifugal defoaming treatment by a defoaming instrument to obtain the required low-foam graphene slurry. The graphene slurry prepared by the method has the advantages of good stability, high uniformity, few graphene defects, thin sheet layer and adjustable sheet diameter. The device simple operation, difficult raise dust and safe and reliable are applicable to full-line automation large-scale production graphite alkene thick liquids.
Description
Technical Field
The invention relates to a device and a method for industrially and continuously preparing graphene slurry, which are suitable for the engineering preparation of nano materials and belong to the technical field of nano materials.
Background
Since 1840 the advent of graphene, the two-dimensional material was successively found to be highConductivity, high electron mobility: (>2×105cm2·V-1·s-1) High thermal conductivity (>3000 W·mK-1) High Young's modulus: (>0.5-1 TPa), high elastic coefficient (1-5 N.m)-1) And the experimental value is as high as 400-700m2·g-1Specific surface area of (2). Graphene has been exposed in various fields such as functional coatings, heat-conducting and heat-dissipating materials, composite photoelectric materials, energy storage, biological photoelectric devices, biomarkers, catalysts and the like.
Due to the problems of easy agglomeration and difficult dispersion of graphene powder, the slurry obtained by dispersing the graphene powder in a corresponding solvent is used for downstream application. However, the high price of graphene is limited, and a safe preparation process of graphene slurry with low cost, batch production, few defects, high dispersibility, stability and leveling property is urgently needed to be developed.
Common stripping methods for graphite raw materials include a hot intercalation method, a microwave method, an acid oxidation intercalation method and the like, and the methods all can cause damage to a graphite lamellar structure, more defects and reduced quality, are not suitable for application in the fields of corrosion prevention, heat conduction and heat dissipation, energy storage and the like, and have the problems of dust emission and explosion. Physical methods such as a ball milling method, a sand milling method, high-speed shearing and the like which can be adopted for reducing defects are mostly batch preparation methods, separation of grinding balls and the like are involved in post-treatment, manual repeated operation is needed, and manpower and material resources are consumed. In addition, the ultrasonic method serving as a mild large-batch graphene stripping method still has the defects of single frequency and power and long preparation time. Particularly, the sounder is in direct contact with the slurry, the metal material slowly permeates into the slurry to cause pollution, and the hidden danger of equipment corrosion is not a little great deal. In response to the requirements of conductive, heat-dissipating, wear-resistant materials and the like, the graphene slurry needs to have good leveling property, and the coating has no obvious bubbles and good adhesion. The tiny bubbles generated in the conventional preparation process are difficult to completely remove, and the application performance of the defoaming agent can be influenced by introducing a sufficient amount of the defoaming agent. Therefore, it is an urgent problem to develop a production apparatus or method for continuously preparing graphene slurry, which can be used for industrial production.
Disclosure of Invention
The invention aims to overcome the defects of the existing graphene slurry preparation process and provide a device and a method for industrially and continuously preparing graphene slurry. The device is in full-line automatic production, convenient to operate, not easy to raise dust, safe and reliable.
The above object of the present invention is mainly achieved by the following technical solutions:
the utility model provides a device of graphite alkene thick liquids is prepared in succession in industrialization, includes liquid nitrogen roll-in appearance, stirred tank, supersound pipeline and removes the bubble appearance, liquid nitrogen roll-in appearance grinds the chamber including the liquid nitrogen roller that inside set up, liquid nitrogen roller grinds chamber one end and sets up the feed inlet, and the bottom of the other end sets up the discharge gate, liquid nitrogen roller grinds intracavity portion and is provided with the grinding roller of staggered arrangement, liquid nitrogen roller grinds chamber bottom and sets up the material conveyer belt, the material conveyer belt in discharge gate department with stirred tank's entry butt joint, stirred tank's export pass through pipeline and delivery pump with the entry linkage of supersound pipeline, the supersound pipeline includes the cooling frame, sets up the pipeline on the cooling frame and sets up the supersound oscillator on the pipeline, the export of supersound pipeline is connected with removing the bubble.
Further, the ultrasonic bubble remover also comprises a liquid storage tank, wherein an inlet of the liquid storage tank is connected with an outlet of the ultrasonic pipeline, and an outlet of the liquid storage tank is connected with the bubble remover.
Further, remove the bubble appearance including fixed shell, the inside rotatory inner bag that is provided with of fixed shell, rotatory inner bag pass through swivel bearing with fixed shell connects, the last bubble separator tube that is provided with of swivel bearing, the bubble separator tube is provided with a plurality of gas pockets, be provided with on the lateral wall of rotatory inner bag and hinder the bubble mesh hole, there is the interval between rotatory inner bag and the fixed shell in removing the bubble appearance, the material export that removes the bubble appearance set up in on the fixed shell in the interval, the material entry with the inside being linked together of rotatory inner bag, the material entry with the exit linkage of liquid storage pot.
Furthermore, the bubble separation pipe is provided with a flow blocking blade along the axial direction and is connected with a vacuum pump.
Furthermore, a first automatic metering feeding trough is arranged at one end of a feeding hole of the liquid nitrogen roller pressing instrument, and a discharging hole of the first automatic metering feeding trough is connected with the feeding hole.
Furthermore, a support frame is arranged below the liquid nitrogen roller pressing instrument.
Furthermore, the inlet of the stirring kettle is an inclined opening arranged on the side surface and used for receiving materials conveyed by the material conveying belt.
Further, a second automatic metering feeding groove is arranged at the top end of the stirring kettle.
Furthermore, a material transmission connecting assembly is arranged at an inlet of the stirring kettle, one end of the material transmission connecting assembly is in butt joint with the material conveying belt, and the other end of the material transmission connecting assembly is in butt joint with the stirring kettle.
Still further, material transmission coupling assembling includes conveyer belt and big inclination smooth surface slope of interconnect, wherein the conveyer belt butt joint the material conveyer belt, big inclination smooth surface slope butt joint the entry of stirred tank.
Further, the outlet of the liquid storage tank is connected with a bubble removing instrument through a material pump.
Further, a liquid nitrogen cooling layer is arranged on the periphery of the cavity body adjacent to the liquid nitrogen roller grinding cavity, and the liquid nitrogen cooling layer has a hollow structure, and the inside of the hollow structure can be filled with liquid nitrogen. Further, the liquid nitrogen cooling layer can continuously pass through liquid nitrogen. And a liquid nitrogen heat insulation layer is arranged on the outer side of the liquid nitrogen cooling layer, and a low-temperature heat insulation material is contained in the liquid nitrogen heat insulation layer.
Further, a liquid level alarm is arranged at the feed inlet.
Furthermore, the liquid level alarm is an infrared liquid level alarm.
Further, the grinding roller is a cylindrical roller shaft, the roller shaft is made of low-temperature-resistant and wear-resistant materials, the surface of the roller shaft is a smooth surface or is provided with dislocation ripples, and the dislocation angle of the adjacent roller shafts is 10-80 degrees; furthermore, the diameter of the roller shaft can be 20-100mm, and the length can be 100-1000 mm.
Furthermore, the grinding roller can be provided with more than two layers, so that the grinding effect is better realized; furthermore, different grinding directions can be adopted between adjacent layers, and then the multi-angle grinding is guaranteed to achieve a better grinding effect.
Further, the bottom of the stirring kettle is provided with a weighing module, a cleaning spraying ball is arranged above the inside of the stirring kettle, and a stirrer is arranged inside the stirring kettle.
Furthermore, the cooling frame is three-dimensional, heat exchange media are filled in the cooling frame, the pipelines are arranged in an S shape, a plurality of ultrasonic vibrators are uniformly distributed on the outer wall of each pipeline, the S-shaped elbows of the pipelines are tightly attached and fixed to the cooling frame, and the ultrasonic vibrators are not arranged at the elbows; the cooling rack is internally provided with a temperature probe, and the side surface or the top of the cooling rack is provided with a temperature display connected with the temperature probe.
Furthermore, the cooling rack is a three-dimensional cuboid, the pipelines can be arranged along the cooling rack in the horizontal direction or the vertical direction, the cross section of each pipeline can be in a chamfered cube shape, and the side length can be 30-500 mm; the two adjacent ultrasonic vibrators are sequentially arranged in an equiangular staggered manner, the staggered angle between the two adjacent ultrasonic vibrators can be 10-75 degrees, the frequency of a single ultrasonic vibrator can be 15-60kHz, and the power can be 20-200W.
The method for preparing the graphene slurry by the device for industrially and continuously preparing the graphene slurry comprises the following steps:
step 1, putting graphite, a first auxiliary agent and liquid nitrogen into a liquid nitrogen roller grinding cavity together, grinding and pre-intercalating through a grinding roller to obtain a pre-grinding material, and outputting the pre-grinding material to a stirring kettle through a material conveying belt;
step 2, adding a second auxiliary agent and a solvent into the pre-ground material in the stirring kettle, and stirring to obtain a mixture;
step 3, conveying the mixture to an ultrasonic pipeline, and dispersing the mixture in the pipeline of the ultrasonic pipeline under the ultrasonic action of an ultrasonic vibrator to obtain a graphene dispersion liquid;
and 4, sending the graphene dispersion liquid into a defoaming instrument for defoaming treatment to obtain graphene slurry.
Further, the graphite in the step 1 comprises crystalline flake graphite, microcrystalline graphite, single crystal graphite,One or a combination of at least two of nano graphite powder, pyrolytic graphite, graphite fluoride or graphene micro-sheets, and the like, preferably crystalline flake graphite, microcrystalline graphite, nano graphite powder, pyrolytic graphite and graphite fluoride; the first auxiliary agent comprises carbon fibers, conductive graphite powder, carbon black, carbon nano tubes and TiO2One or a combination of at least two of silver powder and the like; the mass flow ratio of the first auxiliary agent to the graphite is 1:20-7:10, preferably 1:5-1: 2.
Further, the mass flow ratio of the graphite to the liquid nitrogen in the step 1 is 1:20-1:500, and preferably, the mass flow ratio of the crystalline flake graphite to the liquid nitrogen is 1: 50; preferably, the mass flow ratio of the microcrystalline graphite to the liquid nitrogen is 1: 80; preferably, the mass flow ratio of the pyrolytic graphite to the liquid nitrogen is 1: 160; preferably, the mass flow ratio of the graphene nanoplatelets to the liquid nitrogen is 1: 370.
Further, in the step 1, the dislocation angle of adjacent roll shafts of the grinding roll is 25-60 degrees, and the rotating speed is 20-80 mm/s; the material transfer rate is preferably 100-.
Further, the solvent in step 2 comprises one or a combination of at least two of water, ethanol, terpineol, NMP and the like; the mass flow ratio of the second auxiliary agent to the graphite is 3:100-1: 2; the second auxiliary agent comprises one or the combination of at least two of a dispersing agent, a flatting agent, a film forming agent and a defoaming agent; the stirring speed is 2500-15000r/min, preferably 5000 r/min.
Furthermore, in the step 3, each section of straight pipeline between the cooling racks is regarded as a pipeline unit, the pipeline units are sequentially numbered from the feeding end to the discharging end, and the total power of the vibrators on the horizontal plane of each pipeline unit or each pipeline is in a function, index or linear corresponding relation with the serial number of the pipeline unit. Preferably, the total power of the pipeline units or planes is in a functional corresponding relation with the serial numbers, and more preferably, the functional relation is quadratic. The frequency of the vibrator is not changed, or the vibrator can be sequentially increased or decreased along with the serial number of the pipeline unit.
Compared with the prior art, the device and the method for industrially and continuously preparing the graphene slurry have the following beneficial effects:
1. the liquid nitrogen roller mill provided by the invention is provided with the row-connected roller shafts, can treat graphite in batch, avoids repeated manual operation required by single-kettle ball milling, and has high treatment efficiency. Through physical grinding, the graphene lamellar structure is kept complete, and the problems of multiple defects easily caused by acid, heat, microwave and other treatments are avoided. Adopt upper and lower floor's liquid nitrogen intermediate layer and outer insulating layer to keep warm, the liquid nitrogen rate of volatilizing that slows down need not to supply the liquid nitrogen many times, and the discharge gate powder is slightly wet, is difficult for the raise dust, simple operation and safe and reliable.
2. The graphite and the first auxiliary agent are simultaneously ground in the liquid nitrogen roller mill, so that the graphite and the first auxiliary agent can be simultaneously embrittled and are N-coated2The first auxiliary agent is immediately filled or adsorbed at the edge of the intercalated graphite, and the first auxiliary agent and the graphite form a high-binding-degree microstructure, so that the stability and uniformity of the slurry can be enhanced.
3. The ultrasonic pipeline provided by the invention can fully utilize the field space, adjust the power through a function, an index or a linear relation, and adapt to the energy required by graphene stripping and sheet layer fracture in different ultrasonic stages and the optimal energy corresponding to slurries with different viscosities; the frequency is adjusted in an increasing or decreasing mode, so that the change of the viscosity of the slurry and the change of the graphene interlayer distance in the front and back ultrasonic stages are adapted. The ultrasonic source with the external vibrator can effectively avoid the corrosion of the feed liquid to the sounding source, thereby ensuring that the slurry has no infiltration pollution and prolonging the service life of the ultrasonic equipment.
4. According to the invention, the flow of the slurry is buffered by the liquid storage tank, and the slurry is defoamed by the defoaming instrument, so that the prepared graphene slurry has few bubbles and good stability.
Drawings
Fig. 1 is a schematic view of an apparatus for industrially and continuously preparing graphene slurry according to embodiment 1 of the present invention;
fig. 2 is a transmission electron microscope microstructure view of 7000 times of magnification of the graphene slurry prepared in embodiment 3 of the present invention;
in the above fig. 1, 1 is a liquid nitrogen roller instrument, 11 is a liquid nitrogen roller grinding chamber, 111 is a feed inlet, 112 is a discharge outlet, 113 is a grinding roller, 114 is a material conveyer belt, 12 is a first automatic metering feeding trough, 13 is a liquid nitrogen cooling layer, 14 is a liquid level alarm, 15 is a liquid nitrogen heat-insulating layer, 16 is a support frame, 2 is a stirring kettle, 21 is a second automatic metering feeding trough, 22 is a weighing module, 23 is a cleaning spray ball, 24 is a stirrer, 25 is a material transmission connecting assembly, 3 is an ultrasonic pipeline, 31 is a cooling frame, 32 is a pipeline, 33 is an ultrasonic vibrator, 34 is a temperature probe, 35 is a temperature display, 4 is a liquid storage tank, 5 is a bubble removing instrument, 51 is a fixed shell, 52 is a rotating inner container, 53 is a rotating bearing, 54 is a bubble separating pipe, 55 is a bubble blocking mesh, 56 is a material outlet, 57 is a material inlet, 58 is a flow blocking blade, 6 is a conveying pump, 7 is a material pump, and 8 is a vacuum pump.
The specific implementation mode is as follows:
in order to make the technical problems, technical solutions and advantageous effects solved by the present invention clearer, the present invention is further described in detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Example 1
The embodiment provides a device for industrially and continuously preparing graphene slurry, as shown in fig. 1, the device comprises a liquid nitrogen roller mill 1, a stirring kettle 2, an ultrasonic pipeline 3, a liquid storage tank 4 and a bubble removal instrument 5, wherein the liquid nitrogen roller mill 1 comprises a liquid nitrogen roller mill cavity 11 arranged inside, one end of the liquid nitrogen roller mill cavity 11 is provided with a feed inlet 111, the bottom of the other end is provided with a discharge outlet 112, grinding rollers 113 arranged in a staggered manner are arranged inside the liquid nitrogen roller mill cavity 11, the bottom of the liquid nitrogen roller mill cavity 11 is provided with a material conveyer belt 114, the material conveyer belt 114 is butted with an inlet of the stirring kettle 2 at the discharge outlet 112, an outlet of the stirring kettle 2 is connected with an inlet of the ultrasonic pipeline 3 through a pipeline and a conveying pump 6, the ultrasonic pipeline 3 comprises a cooling frame 31, a pipeline 32 arranged on the cooling frame 31 and an ultrasonic vibrator 33 arranged on the pipeline 32, an outlet of the ultrasonic pipeline 3 is connected with an inlet, the bubble removing instrument 5 comprises a fixed shell 51, a rotary inner container 52 is arranged inside the fixed shell 51, the rotary inner container 52 is connected with the fixed shell 51 through a rotary bearing 53, a bubble separating tube 54 is arranged on the rotary bearing 53, the bubble separating tube 54 is provided with a plurality of air holes, a bubble blocking mesh hole 55 is arranged on the side wall of the rotary inner container 52, an interval exists between the rotary inner container 52 and the fixed shell 51 in the bubble removing instrument 5, a material outlet 56 of the bubble removing instrument 5 is arranged in the interval, a material inlet 57 is communicated with the inside of the rotary inner container 52, the material inlet 57 can be arranged at the central position of the rotary inner container 52 in the axial direction of rotation, if the position of the rotary bearing 53 is right opposite, so as to ensure the normal use of the material inlet 57 and not rotate along with the inner container. The material inlet 57 is connected with the outlet of the liquid storage tank 4.
Further, a support frame 16 is arranged below the liquid nitrogen roller pressing instrument 1.
Further, the liquid nitrogen roller pressure instrument 1, the stirring kettle 2, the ultrasonic pipeline 3, the liquid storage tank 4 and the bubble removing instrument 5 all comprise explosion-proof devices.
Further, a first automatic metering feeding groove 12 is arranged at one end of a feeding hole 111 of the liquid nitrogen roller pressure instrument 1, and a discharging hole of the first automatic metering feeding groove 12 is connected with the feeding hole 111.
Further, a second automatic metering feeding groove 21 is arranged at the top end of the stirring kettle 2.
Further, the outlet of the liquid storage tank 4 is connected with a bubble removing instrument 5 through a material pump 7.
Further, a liquid nitrogen cooling layer 13 is arranged on the periphery of the cavity adjacent to the liquid nitrogen roller grinding cavity 11, and the liquid nitrogen cooling layer 13 has a hollow structure capable of being filled with liquid nitrogen.
Further, a liquid level alarm 14 is arranged at the feed port 111, and preferably, an infrared liquid level alarm can be selected.
Further, 2 bottoms of stirred tank set up weighing module 22, stirred tank 2 is inside to be provided with the washing and sprays ball 23 in the top, stirred tank 2 is inside to set up agitator 24.
Further, the cooling frame 31 is three-dimensional, and heat exchange medium is filled to the inside, pipeline 32 is the S type and arranges, ultrasonic vibrator 33 quantity is a plurality of, evenly arranges on pipeline 32, and the equal angle dislocation is arranged in order between two adjacent ultrasonic vibrator 33, cooling frame 31 inside can be provided with a plurality of temperature probe 34, and a plurality of temperature probe 34 are connected with temperature display 35 and are shown the test temperature.
Further, a flow blocking vane 58 is axially arranged on the bubble separation pipe 54, and the bubble separation pipe 54 is connected with the vacuum pump 8.
Further, the number of the first automatic metering feeding grooves 12 arranged at one end of the feeding port 111 of the liquid nitrogen roller instrument 1 is at least three, one is a liquid nitrogen groove with the inflow rate controlled by a liquid nitrogen tank through an electromagnetic valve, the other is a graphite groove with the graphite powder vibration controlled amount fed, the third is a feeding groove of the first auxiliary agent, and the feeding grooves include but are not limited to the three. Furthermore, the data of the first automatic metering feeding trough 12 can be collected and connected to an electric control system, and the flow rate of each material can be input and set by an operation panel of the control system. A smooth surface inclination angle is arranged at the position of a feeding hole 111 right below a discharging hole of the first automatic metering charging groove 12, an infrared liquid level alarm is arranged at the position of a feeding slope of the smooth surface inclination angle, and the liquid nitrogen liquid level is sent out to give an alarm when the infrared detection temperature is lower than a set value. Furthermore, signals can be transmitted to the control system, and the feed flow of each material can be regulated and controlled by feedback signals.
Further, the grinding roller 113 is a cylindrical roller shaft arranged in a staggered manner, the roller shaft is made of low-temperature-resistant and wear-resistant materials, the surface of the roller shaft is smooth or has staggered corrugations, the diameter of the roller shaft is 20-100mm, the length of the roller shaft is 100-1000mm, and the staggered angle of the adjacent roller shafts is 10-80 degrees. The roller shafts are horizontally vertical to the material conveying direction, and the vertical direction and the horizontal direction are both formed by multiple layers of roller shafts. The roll shafts can also be vertically vertical to the material conveying direction, the vertical direction is composed of two or more roll shafts, the highest position of the roll shafts is slightly lower than the lower edge of the liquid nitrogen cooling layer 13, and the horizontal direction is composed of at least one layer of roll shaft. A material conveying belt 114 is arranged below the roller shaft, and the conveying direction is from the feeding groove end to the stirring kettle 2 end.
Further, the liquid nitrogen cooling layer 13 can be distributed around the liquid nitrogen roller grinding cavity 11, liquid nitrogen continuously passes through the liquid nitrogen cooling layer 13, and the flow direction of the liquid nitrogen on the layer is opposite to the material transmission direction and is used for slowing down the volatilization rate of the liquid nitrogen in the liquid nitrogen roller grinding cavity 11.
Further, a liquid nitrogen heat insulation layer 15 is arranged on the periphery of the liquid nitrogen cooling layer 13 and contains a low-temperature heat insulation material, so that volatilization of liquid nitrogen in the liquid nitrogen cooling layer can be reduced.
Further, a material transmission connection assembly 25 is arranged at an inlet of the stirring kettle 2, one end of the material transmission connection assembly is in butt joint with the material conveying belt 114, and the other end of the material transmission connection assembly is in butt joint with the stirring kettle 2.
Still further, material transmission coupling assembling includes conveyer belt and big inclination smooth surface slope of interconnect, wherein the conveyer belt butt joint the material conveyer belt, big inclination smooth surface slope butt joint the entry of stirred tank.
Furthermore, the support frame 16 contains grounding means to prevent static buildup during the roller milling process.
Furthermore, a confluence transmission device can be added at the discharge port 112 of the liquid nitrogen roller mill 1, so that materials at the discharge ports 112 of at least two liquid nitrogen roller mills 1 are converged into the confluence transmission device and are thrown into the stirring kettle 2 through the material transmission connection assembly 25, thereby increasing the productivity.
Furthermore, a shunt transmission device can be added at the discharge port 112 of the liquid nitrogen roller press 1, and the aim of circulating the feed back roller mill to enhance the roller mill effect is achieved by closing the material transmission connection assembly 25 flowing to the stirring tank 2 and opening the shunt transmission device flowing to the feed port 112 of the roller press 1.
Further, the stirrer 24 may have a central axis in a vertical direction or an inclined direction, and the second automatic metering and feeding tanks 21 may be distributed around the stirrer. The weighing module 22 can calculate the pre-grinding material feeding flow through the total mass change in the stirring kettle 2 in unit time, and further can regulate and control the ratio of the pre-grinding material feeding flow to the material in the upper feeding groove.
Further, in the ultrasonic pipeline 3, the pipeline 32 is S-shaped, and is spread vertically upward for a turning distance after spreading along the horizontal direction, and is spread horizontally again to form a required rectangular structure in sequence. Each straight pipeline is regarded as a pipeline unit, and each semicircular ring is regarded as a pipeline elbow. 2-200 pipeline units in the horizontal direction and the vertical direction of the pipeline can be respectively arranged and can be adjusted according to the planning of the workshop position; the pipeline section can be in a chamfer cube shape, and the side length can be 30-500 mm.
Furthermore, in the ultrasonic pipeline 3, the ultrasonic vibrator 33 is a surrounding type ultrasonic vibrator, the surrounding type ultrasonic vibrator is attached to the outer wall of the pipeline unit, and the vibrator is not arranged at the elbow of the pipeline. The adjacent two ultrasonic vibrators are sequentially staggered at equal angles, and the staggered angle between the adjacent ultrasonic vibrators is 10-75 degrees; the frequency of a single ultrasonic vibrator is 15-60kHz, and the power is 20-200W; each cubic surface of the pipeline unit contains 1-10 ultrasonic vibrators, and the power or frequency of the ultrasonic vibrators of different pipeline units can be consistent or inconsistent.
Furthermore, in the ultrasonic pipeline 3, the cooling frame 31 is of a vertical cuboid structure, contains a heat exchange medium inside, controls the temperature of the materials inside the pipe at the turning position, and supports the weight of the pipe.
Further, an outlet arranged at the bottom of the liquid storage tank 4 is connected with the bubble removing instrument 5 through a material pump 7 and a pipeline. The liquid storage tank 4 plays a role in buffering feed liquid for feeding of the bubble removing instrument 5; furthermore, a stirrer can be arranged at the upper part of the liquid storage tank 4, a pump can be additionally arranged between the inlet and the ultrasonic pipeline 3, and a weighing module can be arranged at the bottom.
Further, the central position below the fixed shell 51 of the bubble removing instrument 5 is a material inlet 57, and one side above the fixed shell is provided with a material outlet 56. The side wall of the bubble separation pipe 54 is provided with air holes, and the periphery of the bubble separation pipe is provided with flow blocking blades 58. The vacuum pump 8 is connected to a bubble separation tube 54. The liquid material is fed through the material inlet 57, flows peripherally in the rotating inner container 52 by centrifugal force, flows through the flow blocking vanes 58 of the bubble separating tube 54 and the bubble blocking meshes 55 of the inner container wall to the space between the rotating inner container 52 and the fixed casing 51, and flows out through the upper material outlet 56. The negative pressure generated by the vacuum pump 8 discharges the bubbles adhering to the bubble separation tube 54. Wherein, the liquid inlet speed, the rotating speed of the rotating liner, the angle of the flow blocking blades and the size of the foam blocking mesh can be adjusted according to the viscosity and the granularity of the material.
Example 2
Based on the apparatus for industrially and continuously preparing graphene slurry described in the above embodiment 1, this embodiment provides a method for industrially and continuously preparing graphene slurry, which includes the steps of:
step 1, pre-intercalation grinding: continuously adding graphite and a first auxiliary agent into a liquid nitrogen flow by a first automatic metering feeding groove, grinding and pre-intercalating the mixture by a grinding roller in a liquid nitrogen roller grinding cavity, regulating and controlling a grinding process by controlling material ratio, the number of roller shafts, rotating speed, arrangement mode and transmission rate to obtain a pre-grinding material, and outputting the pre-grinding material to a stirring kettle by a material conveyer belt;
step 2, stirring and mixing: the ratio of the pre-grinding material, the second auxiliary agent and the solvent is regulated and controlled by controlling the feeding rate of a second automatic metering feeding groove at the top of the stirring kettle, and the mixture is obtained by stirring and mixing at a high speed;
step 3, ultrasonic dispersion: pumping the mixture into an ultrasonic pipeline, and controlling the ultrasonic stripping effect by regulating and controlling the number of ultrasonic vibrators, power, frequency, the number of pipeline units, flow rate and other factors to obtain graphene dispersion liquids with different specifications;
step 4, removing bubbles: and buffering the graphene dispersion liquid by a liquid storage tank, and performing centrifugal defoaming treatment by a defoaming instrument to obtain the required low-foam graphene slurry.
Further, in the above preparation method, the graphite in step 1 includes one or a combination of at least two of flake graphite, microcrystalline graphite, single crystal graphite, nano graphite powder, pyrolytic graphite, fluorinated graphite, graphene nanoplatelets, and the like, preferably flake graphite, microcrystalline graphite, nano graphite powder, pyrolytic graphite, and fluorinated graphite, and more preferably flake graphite, nano graphite powder, and pyrolytic graphite. Furthermore, the graphite can be soaked in liquid nitrogen for a certain time in advance before being fed into the liquid nitrogen roller mill.
Further, in the step 1, the first auxiliary agent comprises carbon fiber, conductive graphite powder, carbon black, carbon nano tube and TiO2And silver powder, or a combination of at least two of them, preferably conductive graphite powder, carbon black, and carbon nanotubes.
Further, the mass flow ratio of the first auxiliary agent to the graphite in the step 1 is 1:20-7:10, preferably 1:5-1: 2.
Further, the first auxiliary agent may not be contained in the step 1.
Further, a dispersant may be contained in step 1.
Further, the mass flow ratio of the graphite to the liquid nitrogen in the step 1 is 1:20-1:500, and preferably, the mass flow ratio of the crystalline flake graphite to the liquid nitrogen is 1: 50; preferably, the mass flow ratio of the microcrystalline graphite to the liquid nitrogen is 1: 80; preferably, the mass flow ratio of the pyrolytic graphite to the liquid nitrogen is 1: 160; preferably, the mass flow ratio of the graphene nanoplatelets to the liquid nitrogen is 1: 370.
Further, in the step 1, preferably, the roll shafts are horizontally vertical to the material conveying direction, the roll shafts in the horizontal direction are 3-8m in total length, the roll shafts in the vertical direction are 3-10 layers in total height, the dislocation angle of adjacent roll shafts is 25-60 degrees, and the rotating speed is 20-80 mm/s; the material transfer rate is preferably 100-.
Further, the solvent in step 2 includes one or a combination of at least two of water, ethanol, terpineol, NMP, and the like.
Further, in the step 2, the second auxiliary agent includes one or a combination of at least two of a dispersant, a leveling agent, a film forming agent, a defoaming agent and the like.
Furthermore, the dispersing agent comprises one or the combination of at least two of sodium deoxycholate, fatty alcohol-polyoxyethylene ether, sodium polynaphthalene formaldehyde sulfonate, sodium N-benzyl-2-heptadecyl benzimidazole sulfonate, tween T-80 and the like;
further, the leveling agent comprises one or two of polyacrylate and modified organic siloxane; the film forming agent comprises one or two of polyvinyl alcohol, polyquaternium and the like; the defoaming agent comprises one or two of polyether modified organic silicon defoaming agent, high-alcohol defoaming agent and the like; this is by way of example and not limitation.
During implementation, the mass flow ratio of the second auxiliary agent to the graphite can be 3:100-1:2, the preferable ratio for preparing the conductive graphene slurry is 1:10-1:5, and the preferable ratio for preparing the graphene slurry for heat conduction and heat dissipation is 2: 5.
Further, in step 2, the stirring speed of the stirring kettle may be 2500-.
Furthermore, in the step 3, each section of the straight pipeline is regarded as a pipeline unit, the pipeline units are sequentially numbered from the feeding end to the discharging end, and the total power of the vibrators on each pipeline unit or each pipeline horizontal plane and the serial number of the pipeline unit are in a function, index or linear corresponding relation. The linear correspondence includes the conditions of oscillator arrangement, positions and total power consistency.
Preferably, the total power of the pipeline units or planes is in a functional corresponding relation with the number, and more preferably in a quadratic function relation.
Further, for slurry with low solid content or low viscosity of graphene, an ultrasonic mode of gradually changing from low power to high power can be adopted for dispersion; and for slurry with high solid content, high viscosity or poor fluidity of graphene, the graphene can be dispersed in a mode of descending ultrasonic power.
When the ultrasonic vibrator frequency is implemented, the frequency of the ultrasonic vibrator can be sequentially increased or decreased progressively along with the serial number of the pipeline unit, also can be fixed as a value, and also can be gradually increased or decreased progressively.
Example 3
The embodiment provides a method for industrially and continuously preparing graphene slurry based on embodiment 2, which includes the following steps:
step 1, pre-intercalation grinding: injecting liquid nitrogen into the liquid nitrogen feeding groove for pre-cooling, and controlling the mass flow ratio of the crystalline flake graphite, the carbon nano tube and the liquid nitrogen in the first automatic metering feeding groove to be 5:1: 250. The mixture enters a liquid nitrogen roller grinding cavity to be ground and pre-intercalated. The roller of grinding roller and material transmission direction level are perpendicular, diameter 50mm, length 200mm, and the surperficial plain noodles, horizontal direction roller 6m total length, 4 layers of total height on vertical direction roller, and adjacent roller dislocation angle is 45, and the rotational speed is 40 mm/s. The mixture material is output by a material conveyer belt and is conveyed into a stirring kettle, and the output speed of the material conveyer belt is 350 mm/min;
step 2, stirring and mixing: solvent water, a dispersing agent N-benzyl-2-heptadecyl benzimidazole sodium sulfonate, film forming agent polyvinyl alcohol and an organic silicon defoaming agent are added into a stirring kettle from a second automatic metering feeding groove, and a mixture is obtained by stirring at the rotating speed of 5000r/min, wherein the feeding mass flow ratio of the pre-grinding agent, the dispersing agent, the film forming agent and the defoaming agent is 300:40:25: 9.
Step 3, ultrasonic dispersion: pumping the mixture into an ultrasonic pipeline, wherein the pipeline comprises 10 pipeline units in the horizontal direction, 10 pipeline units in the vertical direction and 100mm side length of the pipeline, and adjacent ultrasonic vibrationThe dislocation angle between the sub-units is 30 degrees, the function relationship between the total power y of the ultrasonic vibrators of the pipeline units and the median x of the serial numbers of the pipeline units is as follows: y is 0.0689x2-1.4917x + 800. Namely, the frequency of a single ultrasonic vibrator is 60kHz within the range of the pipeline number of 1-30, 8 vibrators are arranged on four sides of the pipeline unit respectively, and the power of each ultrasonic vibrator is 25W; in the range of 31-50 pipeline numbers, the frequency of a single ultrasonic vibrator is 40kHz, 6 ultrasonic vibrators are arranged on each of four sides of a pipeline unit, and the power of each ultrasonic vibrator is 35W; in the pipeline number range of 51-75, the frequency of a single ultrasonic vibrator is 40kHz, 7 ultrasonic vibrators are arranged on each of four sides of a pipeline unit, and the power of each ultrasonic vibrator is 35W; in the range of 76-100 pipeline numbers, the frequency of a single ultrasonic vibrator is 28kHz, 6 ultrasonic vibrators are arranged on four sides of the pipeline unit respectively, and the power of each ultrasonic vibrator is 50W. And obtaining the graphene dispersion liquid. The relationship between the ultrasonic vibrator parameter setting and the pipeline number is as follows:
| pipeline numbering | Oscillator frequency/kHz | Number of vibrators per surface | Pipe unit surface/piece | power/W of single oscillator | Total power/W of the range |
| 1-30 | 60 | 8 | 4 | 25 | 800 |
| 31-50 | 40 | 6 | 4 | 35 | 840 |
| 51-75 | 40 | 7 | 4 | 35 | 980 |
| 76-100 | 28 | 6 | 4 | 50 | 1200 |
Step 4, removing bubbles: and buffering the graphene dispersion liquid by a liquid storage tank, and performing centrifugal defoaming treatment by a defoaming instrument to obtain the required low-foam graphene slurry.
As shown in fig. 2, the transmission electron microscope microstructure is 7000 times magnified for the graphene slurry prepared by the above method.
The graphene slurry obtained by the method is coated on a PET substrate, the volume resistivity is measured to be 19.2 mu omega m, the temperature is raised by 5 ℃ within 2min under the low voltage of 5V, and the graphene slurry can be used as a good heat conduction and heat dissipation material and an additive.
Example 4
The embodiment provides a method for industrially and continuously preparing graphene slurry based on embodiment 2, which includes the following steps:
step 1, pre-intercalation grinding: the mass flow ratio of the nano graphite powder, the carbon black and the liquid nitrogen is controlled to be 10:1:720 in the first automatic metering feeding groove. Grinding roller and material transmission direction horizontal vertical in the liquid nitrogen roller mill chamber, diameter 80mm, length 500mm, the roller surface of grinding roller is the symmetry bump, horizontal direction roller 8m total length, vertical direction roller 5 layers total height, and adjacent roller dislocation angle is 60, rotational speed 80 mm/s. The pre-grinding materials are output to the stirring kettle through a material conveying belt, and the material conveying speed of the conveying belt is 200 mm/min.
Step 2, stirring and mixing: and (3) putting the pre-grinding material into a stirring kettle through a material transmission connecting assembly, putting the solvent terpineol into a second automatic metering feeding groove, and stirring at the rotating speed of 3500r/min, wherein the mass flow ratio of the pre-grinding material to the solvent is 7: 93.
Step 3, ultrasonic dispersion: the mixture is pumped into an ultrasonic pipeline, the pipeline comprises 6 pipeline units in the horizontal direction, 12 pipeline units in the vertical direction and 150mm pipeline side length. The dislocation angle between adjacent vibrators is 50 degrees, the frequency of a single ultrasonic vibrator is 20kHz, 10 ultrasonic vibrators are arranged on the four sides of the pipeline unit respectively, the power of each ultrasonic vibrator is 100W, and the graphene dispersion liquid is obtained.
Step 4, removing bubbles: and (3) passing the graphene dispersion liquid through a liquid storage tank and a defoaming instrument to obtain the required low-foam graphene slurry.
The graphene slurry obtained above was coated on a PET substrate, and the volume resistivity was measured to be 12.81 μ Ω · m. The graphene paste and the conductive silver paste are prepared into graphene silver paste according to the mass ratio of 3:7, the volume resistivity is measured to be 2.95 mu omega m, and the graphene paste can be used for manufacturing an RFID chip by silk-screen printing.
Example 5
The embodiment provides a method for industrially and continuously preparing graphene slurry based on embodiment 2, which includes the following steps:
step 1, pre-intercalation grinding: pyrolytic graphite and TiO are controlled to be put into a first automatic metering feeding groove2The mass flow ratio of the powder to the liquid nitrogen is 10:5: 1600. The grinding roller is vertical perpendicular to the material transmission direction in the liquid nitrogen roller grinding cavity, the diameter is 35mm, the length is 100mm, the roller shaft surface of the grinding roller is a fine corrugated surface, the total length of a horizontal roller shaft is 8m, the total height of 1 layer of the vertical roller shaft is 45 degrees, the dislocation angle of adjacent roller shafts is 45 degrees, and the rotating speed is 3 degrees0 mm/s. The pre-grinding materials are output to the stirring kettle through a material conveying belt, and the material conveying speed of the material conveying belt is 150 mm/min.
Step 2, stirring and mixing: and adding the dispersant Tween T-80 and the solvent ethanol into a second automatic metering feeding tank, wherein the mass flow ratio of the pre-grinding material to the dispersant Tween T-80 to the solvent feeding tank is 10:3:87, and stirring at the rotating speed of 8000r/min to obtain a mixture.
Step 3, ultrasonic dispersion: the mixture is pumped into an ultrasonic pipeline, the pipeline comprises 15 pipeline units in the horizontal direction, 10 pipeline units in the vertical direction, and the side length of the pipeline is 65 mm. The dislocation angle between the adjacent ultrasonic vibrators is 20 degrees, and the functional relation between the total power y of the ultrasonic vibrators of the pipeline units and the median x of the serial numbers of the pipeline units is as follows: y is 0.1333x2-24.533x+2125.7(1<x<75)，y＝-13.333x+3106.7(76<x<150). And obtaining the graphene dispersion liquid. The relationship between the ultrasonic vibrator parameter setting and the pipeline number is as follows:
| pipeline numbering | Oscillator frequency/kHz | Number of vibrators per surface | Pipe unit surface/piece | power/W of single oscillator | Total power/W of the range |
| 1-15 | 60 | 8 | 4 | 60 | 1920 |
| 16-30 | 40 | 7 | 4 | 60 | 1680 |
| 31-45 | 40 | 9 | 3 | 50 | 1350 |
| 46-60 | 35 | 6 | 4 | 50 | 1200 |
| 61-75 | 35 | 9 | 3 | 40 | 1080 |
| 76-90 | 28 | 10 | 2 | 100 | 2000 |
| 91-105 | 20 | 9 | 2 | 100 | 1800 |
| 106-120 | 20 | 8 | 2 | 100 | 1600 |
| 121-135 | 15 | 7 | 2 | 100 | 1400 |
| 136-150 | 15 | 6 | 2 | 100 | 1200 |
Step 4, removing bubbles: and (3) passing the graphene dispersion liquid through a liquid storage tank and a defoaming instrument to obtain the required low-foam graphene slurry.
The obtained graphene slurry is added into waterborne polyurethane according to the mass ratio of 1:10, so that the surface roughness of the coating of the obtained composite coating is reduced by 73.2%, the salt water resistance is improved by 55%, and the antibacterial performance is obviously improved. The graphene slurry can be used as a functional modifier of a water-based paint.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are included in the scope of the present invention.
Claims (12)
1. The device for industrially and continuously preparing the graphene slurry is characterized by comprising a liquid nitrogen roller mill (1), a stirring kettle (2), an ultrasonic pipeline (3) and a bubble removal instrument (5), wherein the liquid nitrogen roller mill (1) comprises a liquid nitrogen roller mill cavity (11) which is arranged inside, one end of the liquid nitrogen roller mill cavity (11) is provided with a feed inlet (111), the bottom of the other end of the liquid nitrogen roller mill cavity is provided with a discharge outlet (112), grinding rollers (113) which are arranged in a staggered manner are arranged inside the liquid nitrogen roller mill cavity (11), the bottom of the liquid nitrogen roller mill cavity (11) is provided with a material conveying belt (114), the material conveying belt (114) is in butt joint with an inlet of the stirring kettle (2) at the discharge outlet (112), an outlet of the stirring kettle (2) is connected with an inlet of the ultrasonic pipeline (3) through a pipeline and a conveying pump (6), the ultrasonic pipeline (3) comprises a cooling frame (31), the pipeline (32) arranged on the cooling frame (31) and the ultrasonic vibrator (33) arranged on the pipeline (32), wherein the outlet of the ultrasonic pipeline (3) is connected with the bubble removing instrument (5).
2. The device for the industrial continuous preparation of graphene slurry according to claim 1, wherein a first automatic metering feeding trough (12) is arranged at one end of a feeding hole (111) of the liquid nitrogen roller instrument (1), and a discharging hole of the first automatic metering feeding trough (12) is connected with the feeding hole (111); and a second automatic metering feeding groove (21) is arranged at the top end of the stirring kettle (2).
3. The apparatus for industrially and continuously preparing graphene slurry according to claim 1, wherein a liquid nitrogen cooling layer (13) is arranged on the periphery of the liquid nitrogen roller grinding chamber (11), and the liquid nitrogen cooling layer (13) has a hollow structure of which the interior can be filled with liquid nitrogen.
4. The device for the industrial continuous preparation of graphene slurry according to claim 1, wherein a liquid level alarm (14) is arranged at the feed port (111); the ultrasonic bubble remover is characterized by further comprising a liquid storage tank (4), wherein an inlet of the liquid storage tank (4) is connected with an outlet of the ultrasonic pipeline (3), and an outlet of the liquid storage tank (4) is connected with the bubble remover (5).
5. The device for the industrial continuous preparation of graphene slurry according to claim 1, wherein a weighing module (22) is arranged at the bottom of the stirring kettle (2), a cleaning spray ball (23) is arranged above the inside of the stirring kettle (2), and a stirrer (24) is arranged inside the stirring kettle (2).
6. The device for industrially and continuously preparing graphene slurry according to claim 1, wherein the cooling frame (31) is three-dimensional, heat exchange media are filled in the cooling frame, the pipeline (32) is arranged in an S shape, a plurality of ultrasonic vibrators (33) are uniformly distributed on the outer wall of the pipeline (32), two adjacent ultrasonic vibrators (33) are sequentially arranged in an equiangular staggered manner, S-shaped elbows of the S-shaped arrangement of the pipeline (32) are closely attached to and fixed with the cooling frame (31), the ultrasonic vibrators (33) are not arranged at the S-shaped elbows, a temperature probe (34) is arranged in the cooling frame (31), and a temperature display (35) connected with the temperature probe (34) is arranged on the side surface or the top surface of the cooling frame (31).
7. The device for industrially and continuously preparing graphene slurry according to claim 1, wherein the bubble removing instrument (5) comprises a fixed shell (51), a rotating inner container (52) is arranged inside the fixed shell (51), the rotating inner container (52) is connected with the fixed shell (51) through a rotating bearing (53), a bubble separating tube (54) is arranged on the rotating bearing (53), the bubble separating tube (54) is provided with a plurality of air holes, a bubble blocking mesh (55) is arranged on the side wall of the rotating inner container (52), a gap exists between the rotating inner container (52) and the fixed shell (51) in the bubble removing instrument (5), a material outlet (56) of the bubble removing instrument (5) is arranged on the fixed shell (51) in the gap, and a material inlet (57) is communicated with the inside of the rotating inner container (52), the bubble separation pipe (54) is provided with a flow blocking blade (58) along the axial direction, and the bubble separation pipe (54) is connected with a vacuum pump (8).
8. The device for industrially and continuously preparing the graphene slurry according to claim 3, wherein a liquid nitrogen heat insulation layer (15) is arranged outside the liquid nitrogen cooling layer (13), and the liquid nitrogen heat insulation layer (15) contains a low-temperature heat insulation material.
9. The method for preparing graphene slurry by using the device for industrially and continuously preparing graphene slurry according to claim 1, is characterized by comprising the following steps:
step 1, putting graphite, a first auxiliary agent and liquid nitrogen into a liquid nitrogen roller grinding cavity together, grinding and pre-intercalating through a grinding roller to obtain a pre-grinding material, and outputting the pre-grinding material to a stirring kettle through a material conveying belt;
step 2, adding a second auxiliary agent and a solvent into the pre-ground material in the stirring kettle, and stirring to obtain a mixture;
step 3, conveying the mixture to an ultrasonic pipeline, and dispersing the mixture in the pipeline of the ultrasonic pipeline under the ultrasonic action of an ultrasonic vibrator to obtain a graphene dispersion liquid;
and 4, sending the graphene dispersion liquid into a defoaming instrument for defoaming treatment to obtain graphene slurry.
10. The method according to claim 9, wherein the graphite in step 1 comprises one or a combination of at least two of scale graphite, microcrystalline graphite, single crystal graphite, nano graphite powder, pyrolytic graphite, fluorinated graphite, or graphene micro-sheets, preferably scale graphite, microcrystalline graphite, nano graphite powder, pyrolytic graphite, fluorinated graphite; the first auxiliary agent comprises carbon fibers, conductive graphite powder, carbon black, carbon nano tubes and TiO2Of silver powder and the likeOne or a combination of at least two; the mass flow ratio of the first auxiliary agent to the graphite is 1:20-7:10, preferably 1:5-1: 2; in the step 1, the mass flow ratio of the graphite to the liquid nitrogen is 1:20-1:500, and preferably, the mass flow ratio of the crystalline flake graphite to the liquid nitrogen is 1: 50; preferably, the mass flow ratio of the microcrystalline graphite to the liquid nitrogen is 1: 80; preferably, the mass flow ratio of the pyrolytic graphite to the liquid nitrogen is 1: 160; preferably, the mass flow ratio of the graphene nanoplatelets to the liquid nitrogen is 1: 370.
11. The method according to claim 9, wherein the solvent in step 2 comprises one or a combination of at least two of water, ethanol, terpineol, NMP, and the like; the mass flow ratio of the second auxiliary agent to the graphite is 3:100-1: 2; the second auxiliary agent comprises one or the combination of at least two of a dispersing agent, a flatting agent, a film forming agent, a defoaming agent and the like; the stirring speed is 2500-15000r/min, preferably 5000 r/min.
12. The method according to claim 9, wherein each section of the straight pipeline is regarded as a pipeline unit in the step 3, the pipeline units are numbered sequentially from the feeding end to the discharging end, and the total power of the vibrators on each pipeline unit or each pipeline horizontal plane and the serial number of the pipeline unit are in a function, index or linear corresponding relation; preferably, the total power of the pipeline unit or the plane is in a function corresponding relationship with the serial number, more preferably in a quadratic function relationship, and the frequency of the oscillator is not changed, or can be sequentially increased or decreased along with the serial number of the pipeline unit.
Priority Applications (1)
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| CN201910554515.9A CN112125300A (en) | 2019-06-25 | 2019-06-25 | Device and method for industrially and continuously preparing graphene slurry |
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| CN201910554515.9A CN112125300A (en) | 2019-06-25 | 2019-06-25 | Device and method for industrially and continuously preparing graphene slurry |
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Cited By (3)
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| CN113145283A (en) * | 2021-02-23 | 2021-07-23 | 邯郸钢铁集团有限责任公司 | Laboratory equipment and method for preparing graphene by using tar residues |
| CN113387349A (en) * | 2021-05-12 | 2021-09-14 | 无锡启仁化工科技有限公司 | Method for efficiently preparing graphene sol |
| CN116443865A (en) * | 2023-05-08 | 2023-07-18 | 贺州学院 | Method for preparing graphene from negative electrode graphite of waste lithium ion battery |
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| CN113145283A (en) * | 2021-02-23 | 2021-07-23 | 邯郸钢铁集团有限责任公司 | Laboratory equipment and method for preparing graphene by using tar residues |
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| CN116443865A (en) * | 2023-05-08 | 2023-07-18 | 贺州学院 | Method for preparing graphene from negative electrode graphite of waste lithium ion battery |
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