CN113929932A - Preparation method and preparation equipment applied to carbon nanotube master batch - Google Patents

Preparation method and preparation equipment applied to carbon nanotube master batch Download PDF

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Publication number
CN113929932A
CN113929932A CN202111003256.4A CN202111003256A CN113929932A CN 113929932 A CN113929932 A CN 113929932A CN 202111003256 A CN202111003256 A CN 202111003256A CN 113929932 A CN113929932 A CN 113929932A
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pipe
granulation tower
master batch
carbon nanotube
screen
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CN113929932B (en
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毛鸥
张美杰
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Zhenjiang Xinna Material Technology Co ltd
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Zhenjiang Xinna Material Technology Co ltd
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J3/00Processes of treating or compounding macromolecular substances
    • C08J3/20Compounding polymers with additives, e.g. colouring
    • C08J3/22Compounding polymers with additives, e.g. colouring using masterbatch techniques
    • C08J3/223Packed additives
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29BPREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • B29B13/00Conditioning or physical treatment of the material to be shaped
    • B29B13/06Conditioning or physical treatment of the material to be shaped by drying
    • B29B13/065Conditioning or physical treatment of the material to be shaped by drying of powder or pellets
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29BPREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • B29B13/00Conditioning or physical treatment of the material to be shaped
    • B29B13/10Conditioning or physical treatment of the material to be shaped by grinding, e.g. by triturating; by sieving; by filtering
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29BPREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • B29B9/00Making granules
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00Specific properties of additives
    • C08K2201/011Nanostructured additives
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/02Elements
    • C08K3/04Carbon
    • C08K3/041Carbon nanotubes

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  • Mechanical Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Carbon And Carbon Compounds (AREA)

Abstract

The invention relates to a preparation method and preparation equipment thereof applied to carbon nanotube master batch, wherein the preparation method comprises the steps of pulping, uniformly dispersing carbon nanotube powder with the granularity of 10-150 mu m in a solvent, and ultrasonically stirring for 20min to form slurry; adding a dispersing auxiliary agent, a lubricant and a plasticizer into the slurry, and mechanically stirring for 0.5-1.5 h; putting the final mixed master batch into a slurry grinder to grind for 2-3 h, and filtering by a 50-mesh screen; and finally, putting the filtered slurry into a spray drying granulation tower, spraying the material into a mist state through the spray drying granulation tower, and quickly evaporating and drying to obtain the carbon nano tube master batch. The slurry is prevented from agglomerating, so that fine particles in the slurry reach uniform size, and the conductivity of the carbon nano tube master batch is ensured.

Description

Preparation method and preparation equipment applied to carbon nanotube master batch
Technical Field
The invention belongs to the technical field, and particularly relates to a preparation method and preparation equipment of carbon nanotube master batches.
Background
The carbon nano tube has excellent performances of high strength, high thermal conductivity, high electrical conductivity and the like, has wide potential application prospect in the interdisciplinary fields of material science, chemistry, physics and the like, and is a novel material which draws attention in the 21 st century. Because the high polymer material has high resistivity, static electricity is not easy to remove, accumulated voltage is large, and the production and use processes of plastic products are greatly influenced, and in order to solve the problem, adding the antistatic master batch into the high polymer material is a common solution. At present, the conductive masterbatch of carbon nanotube polymer composite conductive material is prepared by two general methods, one is to melt and blend the polymer material and the carbon nanotube by a double screw extruder or an internal mixer to prepare the conductive masterbatch, the other is to dissolve the polymer material in a solvent, add the carbon nanotube to mechanically stir or ultrasonically disperse, and remove the solvent to prepare the conductive masterbatch.
The existing conductive master batch has poor conductivity, low preparation efficiency and difficult large-scale production. At present, when the carbon nanotube master batch is produced and granulated, a screw extruder is generally adopted to extrude the carbon nanotube master batch into strips and then cut the carbon nanotube master batch into granules, the granule shape of the extruded and granulated product is not round enough, the granule length and the end surface shape can not be accurately controlled, the belt share rate is high, the product quality is difficult to guarantee, the production rate is low, and the carbon nanotube master batch cannot be suitable for large-scale flow line production.
Disclosure of Invention
Aiming at the problems, the invention discloses a preparation method and preparation equipment thereof applied to carbon nanotube master batches, and the preparation method and the preparation equipment are realized.
The specific technical scheme is as follows:
the preparation method of the carbon nanotube master batch is characterized by comprising the following steps:
the method comprises the following steps: pulping, namely uniformly dispersing carbon nanotube powder with the granularity of 10-150 mu m in a solvent, and ultrasonically stirring for 20min to form slurry;
step two: adding a dispersing auxiliary agent, a lubricant and a plasticizer into the slurry, and mechanically stirring for 0.5-1.5 h at the temperature of 30-90 ℃ at the rotating speed of 150-350 rpm;
step three: thinning: putting the final mixed master batch obtained in the step two into a slurry grinder, grinding for 2-3 h, and filtering through a 50-mesh screen;
step four: and (3) spray granulation, namely putting the slurry filtered in the step three into a spray drying granulation tower, spraying the material into a mist shape through the spray drying granulation tower, and quickly evaporating and drying to obtain the carbon nano tube master batch.
The carbon nano tube powder, the solvent, the dispersing auxiliary agent, the lubricant and the plasticizer are prepared from the following components in parts by weight: 10-15: 25-35, 5-10: 1-10: 10 to 15;
in the first step, the solvent comprises one or more of water, ethanol, ethylene glycol, isopropanol, acetone, chloroform, N-methylpyrrolidone, tetrahydrofuran, dimethylformamide and toluene;
and in the fourth step, the raw materials are heated to 100-130 ℃, spray granulation is carried out in a drying chamber with the spray pressure of 0.1-0.5 Mpa at 120-220 ℃, and the hot air temperature is 120-220 ℃.
A preparation device applied to carbon nanotube master batches comprises a granulation tower, a heating device and a material returning device, wherein the heating device is arranged on one side of the granulation tower, the heating device comprises a heater, an air blower and a heating pipe, an air outlet of the air blower is connected with the heater, an air outlet of the heater is connected with the heating pipe, one end of the heating pipe enters the center of the top end of an inner cavity of the granulation tower and is provided with a first air injection pipe orifice, one side of the heating pipe is provided with a branch pipe, one end of the branch pipe horizontally penetrates through the granulation tower and is provided with a second air injection orifice, and the first air injection pipe orifice and the second air injection pipe orifice are arranged in a vertically opposite mode; a feed pipe is arranged at the top end of the granulation tower, one end of the feed pipe longitudinally penetrates through the first air injection pipe opening, and a nozzle is arranged in the first air injection pipe opening;
a discharge hole is formed in the bottom of the granulation tower, a coarse screen assembly, a fine screen assembly and a driving assembly for driving the coarse screen assembly and the fine screen assembly are arranged in an inner cavity of the granulation tower, the coarse screen assembly comprises a coarse screen plate and a stirring impeller, the coarse screen plate is horizontally arranged in the granulation tower, a plurality of coarse screen holes are formed in the coarse screen plate, and the stirring impeller is rotatably arranged in the center of the screen plate; the fine screen component is positioned below the coarse screen component, the fine screen component comprises a screen bucket, a vibrating motor and a material scraping frame, the upper end side wall of the screen bucket is connected with the inner wall of the granulation tower through a plurality of elastic supports, the bottom of the screen bucket is arranged and installed as an inclined plane, one end of the bottom of the screen bucket is obliquely provided with a material conveying pipe, the material conveying pipe penetrates through the granulation tower and is connected with a material returning device, the material returning device is used for conveying particles with smaller sizes into the granulation tower again, the middle part of the screen bucket is horizontally provided with a fine screen plate, the fine screen plate is provided with a plurality of fine screen holes, the screen bucket is positioned at the edge of the side wall of the fine screen plate and is circumferentially provided with a plurality of material discharging ports, the material scraping frame is arranged on the fine screen plate and comprises a fixed seat and a plurality of material scraping rods which are uniformly distributed on the side wall of the fixed seat, the material scraping rods are all arranged in an arc structure, and one end of each material scraping rod extends to the inner wall of the screen bucket, the bottom of each scraping rod is provided with a soft rubber scraping blade; drive assembly is located between coarse screening subassembly and the fine screen subassembly, and drive assembly includes gear box, transmission shaft, driving motor, the gear box sets up at prilling tower inner chamber center, through a plurality of bracing pieces and prilling tower inner wall fixed connection on the lateral wall of gear box upper end, and the gear box is improved level and is run through the setting the transmission shaft, transmission shaft both ends are connected with prilling tower inner wall rotation, and transmission shaft one end is connected with the driving motor output, and driving motor sets up on the prilling tower outer wall and drive the transmission shaft rotatory, the transmission shaft passes through the gear cooperation and drives stirring impeller and scrape the material frame rotatory.
Further, feed back device includes feed back pipe, three solenoid valve, inhales row feed cylinder, rotating electrical machines, lifting unit, the feed back pipe vertically sets up in prilling tower one side, and sets up on the feed back pipe three solenoid valve, three solenoid valve one end with the conveying pipeline is connected, and feed back pipe top is for crooked setting and enter into the prilling tower inner chamber, and the feed back pipe bottom is connected inhale row feed cylinder top, inhale row feed cylinder inner chamber upper end and be equipped with flexible gasbag, flexible gasbag top center is the opening setting, and flexible gasbag bottom is equipped with the lift seat, rotating electrical machines sets up on inhaling row feed cylinder lateral wall, and rotating electrical machines drives the lift seat through lifting unit and goes up and down and compress flexible gasbag to blow in to the prilling tower again in the granule of piling up at the feed back pipe lower extreme.
Further, stirring impeller includes pivot and evenly distributed a plurality of stirring vane in the pivot, stirring vane all is the crooked setting of arc.
Furthermore, the peripheral edge of the fine sieve plate is arranged in an upward inclined manner, and the tail end of the scraping rod is also arranged in an upward bending manner and is matched with the fine sieve plate.
Furthermore, a first bevel gear is arranged on the transmission shaft, a second bevel gear and a third bevel gear are respectively connected to the upper end and the lower end of the first bevel gear in a meshed mode, the second bevel gear and the third bevel gear are respectively arranged on the upper connecting shaft and the lower connecting shaft, the upper connecting shaft and the lower connecting shaft are respectively rotatably arranged at the upper end and the lower end of the gear box, and the upper connecting shaft and the lower connecting shaft are respectively connected with the rotating shaft and the fixing seat.
Furthermore, the lower connecting shaft is connected with the fixed seat through a damping coupler.
Furthermore, a filter screen is arranged in the inner cavity at the lower end of the feed back pipe.
Further, the lifting assembly comprises a rotating disc, a linkage rod and a hinged seat, the rotating disc is longitudinally arranged, the center of the rotating disc is fixedly connected with an output shaft of the rotating motor, protruding seats are symmetrically arranged at two ends of the rotating seat, a fixed shaft is perpendicularly arranged on one of the protruding seats, one end of the linkage rod is rotated on the fixed seat, the other end of the linkage rod is hinged to the hinged seat, and the hinged seat is fixedly arranged at the bottom of the lifting seat.
Furthermore, the lower end of the inner cavity of the suction charging barrel is also provided with a controller and a travel switch, the controller is respectively electrically connected with the travel switch and the three-way electromagnetic valve, and contacts of the travel switch are respectively contacted with the protruding seats at the two ends of the rotating seat, so that the contacts of the travel switch are sequentially pressed through the two protruding seats when the rotating seat rotates.
The invention has the beneficial effects that:
(1) according to the invention, after the slurry is ground by the grinding machine, the slurry is prevented from agglomeration, so that fine particles in the slurry reach uniform size, the subsequent spray granulation is facilitated, the conductivity of the carbon nanotube master batch is ensured, and the roundness of the carbon nanotube master batch is ensured by a spray granulation mode.
(2) According to the invention, the slurry sprayed out of the nozzle is heated and dried by adopting the upper and lower air injection nozzles in the granulation tower, so that the slurry can be quickly evaporated and dried to form spherical particles, the generation of defective products is reduced, the production efficiency is improved, the particles are more uniform after passing through the coarse sieve and the fine sieve in sequence, the particles with smaller size can be filtered, and the production quality of the carbon nano tube master batch is ensured.
(3) The feed back device sucks the small particles and slurry dust discharged by the sieving hopper through the telescopic air bag in the suction and discharge charging barrel and sprays the small particles and the slurry dust into the granulation tower again through the feed back pipe, so that the small particles and the slurry dust can be mixed with each other again to form new particles, the production cost is effectively reduced, and the production quality is further improved.
Drawings
FIG. 1 is a schematic view of a prilling tower according to the present invention.
Fig. 2 is an enlarged schematic view of a point a in fig. 1.
Fig. 3 is a top view of a coarse screen deck according to the present invention.
Fig. 4 is a top view of a fine screen panel according to the present invention.
FIG. 5 is a schematic view showing the structure of the suction/discharge cartridge of the present invention.
Fig. 6 is a schematic structural view of a rotating disk according to the present invention.
The granulating device comprises a granulating tower 1, a discharge hole 11, a heater 2, a blower 21, a heating pipe 22, a branch pipe 221, a first air injection nozzle 222, a second air injection nozzle 223, a feeding pipe 3, a nozzle 31, a coarse screen component 4, a coarse screen plate 41, a coarse screen hole 411, a stirring impeller 42, a rotating shaft 421, stirring blades 422, a fine screen component 5, a screening hopper 51, a feeding pipe 511, a fine screen plate 512, a fine screen hole 5121, a discharge hole 513, a vibrating motor 52, a scraping frame 53, a fixed seat 531, a scraping rod 532, a soft rubber scraping blade 5321, an elastic bracket 54, a driving component 6, a gear box 61, a supporting rod 611, a transmission shaft 62, a first bevel gear 621, a driving motor 63, an upper connecting shaft 64, a second bevel gear 641, a lower connecting shaft 65, a third bevel gear 651, a damping coupling 652, a material returning device 7, a material returning pipe 71, a filtering net 711, a three-way electromagnetic valve 72, a suction and discharge barrel 73, a telescopic air bag 731, a lifting seat 732, a lifting device, a lifting device, a lifting device, a device, The rotary motor 74, the rotary disc 75, the convex seat 751, the fixed shaft 7511, the linkage 76, the hinge seat 77, the controller 78 and the travel switch 79.
Detailed Description
In order to make the technical scheme of the invention clearer and clearer, the invention is further described with reference to the accompanying drawings, and any scheme obtained by carrying out equivalent replacement and conventional reasoning on the technical characteristics of the technical scheme of the invention falls into the protection scope of the invention. The fixing and the arrangement of the fixing and the connection are all general connection modes in the mechanical field, and the fixing and the connection can be performed by welding, bolt and nut connection and screw connection.
In the description of the present invention, it is to be understood that the terms "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", etc. indicate orientations or positional relationships based on those shown in the drawings, and are only for convenience of describing the present invention and simplifying the description, but do not indicate or imply that the referred device or element must have a specific orientation, be constructed in a specific orientation, and be operated, and thus, should not be construed as limiting the present invention.
The preparation method of the carbon nanotube master batch is characterized by comprising the following steps:
the method comprises the following steps: pulping, namely uniformly dispersing carbon nanotube powder with the granularity of 10-150 mu m in a solvent, and ultrasonically stirring for 20min to form slurry;
step two: adding a dispersing auxiliary agent, a lubricant and a plasticizer into the slurry, and mechanically stirring for 0.5-1.5 h at the temperature of 30-90 ℃ at the rotating speed of 150-350 rpm;
step three: thinning: putting the final mixed master batch obtained in the step two into a slurry grinder, grinding for 2-3 h, and filtering through a 50-mesh screen;
step four: and (3) spray granulation, namely putting the slurry filtered in the step three into a spray drying granulation tower, spraying the material into a mist shape through the spray drying granulation tower, and quickly evaporating and drying to obtain the carbon nano tube master batch.
The carbon nano tube powder, the solvent, the dispersing auxiliary agent, the lubricant and the plasticizer are prepared from the following components in parts by weight: 10-15: 25-35, 5-10: 1-10: 10 to 15;
in the first step, the solvent comprises one or more of water, ethanol, ethylene glycol, isopropanol, acetone, chloroform, N-methylpyrrolidone, tetrahydrofuran, dimethylformamide and toluene;
and in the fourth step, the raw materials are heated to 100-130 ℃, spray granulation is carried out in a drying chamber with the spray pressure of 0.1-0.5 Mpa at 120-220 ℃, and the hot air temperature is 120-220 ℃.
A preparation device applied to carbon nanotube master batches comprises a granulation tower 1, a heating device and a material returning device 7, wherein the heating device is arranged on one side of the granulation tower 1 and comprises a heater 2, an air blower 21 and a heating pipe 22, an air outlet of the air blower is connected with the heater 2, an air outlet of the heater 2 is connected with the heating pipe 22, one end of the heating pipe 22 enters the center of the top end of an inner cavity of the granulation tower 1 and is provided with a first air injection pipe orifice 222, one side of the heating pipe 22 is provided with a branch pipe 221, one end of the branch pipe 221 horizontally penetrates through the granulation tower 1 and is provided with a second air injection port, and the first air injection pipe orifice 222 and the second air injection pipe orifice 223 are arranged in a vertically opposite mode; a feed pipe 3 is arranged at the top end of the granulation tower 1, one end of the feed pipe 3 longitudinally penetrates through the first air injection pipe opening 222, and a nozzle 31 is arranged in the first air injection pipe opening 222;
the bottom of the granulation tower 1 is provided with a discharge port 11, a coarse screen component 4, a fine screen component 5 and a driving component 6 for driving the coarse screen component 4 and the fine screen component 5 are arranged in the inner cavity of the granulation tower 1, the coarse screen component 4 comprises a coarse screen plate 41 and a stirring impeller 42, the coarse screen plate 41 is horizontally arranged in the granulation tower 1, a plurality of coarse screen holes 411 are formed in the coarse screen plate 41, and the stirring impeller 42 is rotatably arranged at the center of the screen plate; the fine screen component 5 is located below the coarse screen component 4, the fine screen component 5 comprises a screen hopper 51, a vibration motor 52 and a scraping frame 53, the upper end side wall of the screen hopper 51 is connected with the inner wall of the granulation tower 1 through a plurality of elastic supports 54, the bottom of the screen hopper 51 is arranged and installed on an inclined plane, the vibration motor 52 is obliquely arranged at one end of the bottom of the screen hopper 51, a material conveying pipe 511 is obliquely arranged at one end of the bottom of the screen hopper 51, the material conveying pipe 511 penetrates through the granulation tower 1 and is connected with a material returning device 7, the material returning device 7 is used for re-conveying particles with small sizes to the granulation tower 1, the middle of the screen hopper 51 is horizontally provided with a fine screen plate 512, the fine screen plate 512 is provided with a plurality of fine screen holes 5121, the screen hopper 51 is located at the edge of the side wall of the fine screen plate 512 in the circumferential direction and provided with a plurality of material discharge ports 513, the scraping frame 53 is arranged on the fine screen plate 512, the scraping frame 53 comprises a fixed seat 531 and a plurality of scraping rods 532 evenly distributed on the side wall of the fixed seat 531, the scraping rods 532 are all arranged in an arc structure, one ends of the scraping rods 532 extend to the inner wall of the screening hopper 51, and the bottom of each scraping rod 532 is provided with a soft rubber scraper 5321; a drive assembly 6 is located between the coarse screen assembly 4 and the fine screen assembly 5, the drive assembly 6 comprising a gear box 61, a drive shaft 62, a drive motor 63, the gear box 61 is arranged in the center of the inner cavity of the granulation tower 1, the side wall of the upper end of the gear box 61 is fixedly connected with the inner wall of the granulation tower 1 through a plurality of support rods 611, the transmission shaft 62 is horizontally arranged on the gear box 61 in a penetrating way, two ends of the transmission shaft 62 are rotatably connected with the inner wall of the granulation tower 1, and one end of the transmission shaft 62 is connected with the output end of the driving motor 63, the driving motor 63 is arranged on the outer wall of the prilling tower 1 and drives the transmission shaft 62 to rotate, the transmission shaft 62 drives the stirring impeller 42 and the scraping frame 53 to rotate through the cooperation of the gears, so that the stirring impeller 42 stirs the particles on the coarse sieve plate 41 and makes the particles leak from the coarse sieve holes 411 to the fine sieve plate 512 in the sieving hopper 51, and then the particles with larger sizes are discharged from the discharge port 513 through the rotation of the scraping plate.
Further, the material returning device 7 comprises a material returning pipe 71, a three-way electromagnetic valve 72, a suction and discharge material barrel 73, a rotating motor 74 and a lifting assembly, wherein the material returning pipe 71 is longitudinally arranged on one side of the granulation tower 1, the feed back pipe 71 is provided with the three-way electromagnetic valve 72, one end of the three-way electromagnetic valve 72 is connected with the feed delivery pipe 511, the top end of the feed back pipe 71 is bent and enters the inner cavity of the granulation tower 1, the bottom end of the material return pipe 71 is connected with the top end of the suction and discharge material barrel 73, the upper end of the inner cavity of the suction and discharge material barrel 73 is provided with a telescopic air bag 731, the center of the top end of the telescopic air bag 731 is provided with an opening, the bottom end of the telescopic air bag 731 is provided with a lifting seat 732, the rotating motor 74 is arranged on the side wall of the suction and discharge material barrel 73, and the rotary motor 74 drives the lifting seat 732 to lift and compress the telescopic air bag 731 through the lifting assembly, so that the particles accumulated at the lower end of the feed back pipe 71 are blown into the granulation tower 1 again.
Further, the stirring impeller 42 includes a rotating shaft 421 and a plurality of stirring blades 422 uniformly distributed on the rotating shaft 421, and the stirring blades 422 are all disposed in an arc-shaped curve.
Furthermore, the peripheral edge of the fine sieve plate 512 is inclined upward, and the end of the scraping rod 532 is also bent upward and matched with the fine sieve plate 512.
Further, a first bevel gear 621 is arranged on the transmission shaft 62, a second bevel gear 641 and a third bevel gear 651 are respectively engaged with the upper end and the lower end of the first bevel gear 621, the second bevel gear 641 and the third bevel gear 651 are respectively arranged on the upper connecting shaft 64 and the lower connecting shaft 65, the upper connecting shaft 64 and the lower connecting shaft 65 are respectively rotatably arranged at the upper end and the lower end of the gear box 61, and the upper connecting shaft 64 and the lower connecting shaft 65 are respectively connected with the rotating shaft 421 and the fixing base 531.
Further, the lower connecting shaft 65 is connected with the fixing seat 531 through a damping coupler 652.
Further, a filter screen 711 is arranged in an inner cavity at the lower end of the material return pipe 71.
Further, the lifting assembly comprises a rotating disc 75, a linkage rod 76 and a hinged seat 77, the rotating disc 75 is longitudinally arranged, the center of the rotating disc 75 is fixedly connected with an output shaft of the rotating motor 74, two ends of the rotating seat are symmetrically provided with protruding seats 751, a fixed shaft 7511 is vertically arranged on one of the protruding seats 751, one end of the linkage rod 76 is rotated on the fixed seat 531, the other end of the linkage rod 76 is hinged with the hinged seat 77, and the hinged seat 77 is fixedly arranged at the bottom of the lifting seat 732.
Further, the lower end of the inner cavity of the suction charging barrel 73 is further provided with a controller 78 and a travel switch 79, the controller 78 is electrically connected with the travel switch 79 and the three-way electromagnetic valve 72 respectively, and contacts of the travel switch 79 are in contact with the protruding seats 751 at two ends of the rotating seat respectively, so that the contacts of the travel switch 79 are sequentially pressed through the two protruding seats 751 when the rotating seat rotates, and accordingly the opening of the three-way electromagnetic valve 72 is closed, the three-way electromagnetic valve 72 is located at one end of the material return pipe 71 and is closed, and the three-way electromagnetic valve 72 is located at one end of the material conveying pipe 511 and is closed when the material is sprayed.
The working principle is as follows: the feeding pipe 3 sprays the slurry downwards from the upper end of the granulation tower 1 through the nozzle 31, and simultaneously the first air injection pipe port 222 and the second air injection pipe port 223 blow high-temperature hot air into the granulation tower 1 from the upper end and the lower end respectively, so that the slurry particles are evaporated and dried quickly to form particles, the particles fall downwards into the coarse filter component, the particles are driven to move on the coarse sieve plate 41 through the rotation of the stirring impeller 42 and fall from the coarse sieve pore 411, so that the particles are more uniform, the particles fall downwards onto the fine sieve plate 512 of the sieving hopper 51, the particles are driven to move towards the edge of the fine sieve plate 512 and roll from the discharge port 513 to the bottom end of the granulation tower 1 through the rotation of the scraping frame 53, meanwhile, the particles with small size fall through the fine sieve pore 5121 and fall into the feeding pipe 511 through the vibration effect of the vibration motor 52, the material returning device 7 is driven by the cooperation of the lifting component through the rotation motor 74, so as to realize the suction and discharge of the particles by the material returning pipe 71, so that the fine particles are re-sprayed into the prilling tower 1, so that they can be re-mixed with the slurry and form new particles.
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 also included in the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.

Claims (10)

1. The preparation method of the carbon nanotube master batch is characterized by comprising the following steps:
the method comprises the following steps: pulping, namely uniformly dispersing carbon nanotube powder with the granularity of 10-150 mu m in a solvent, and ultrasonically stirring for 20min to form slurry;
step two: adding a dispersing auxiliary agent, a lubricant and a plasticizer into the slurry, and mechanically stirring for 0.5-1.5 h at the temperature of 30-90 ℃ at the rotating speed of 150-350 rpm;
step three: thinning: putting the final mixed master batch obtained in the step two into a slurry grinder, grinding for 2-3 h, and filtering through a 50-mesh screen;
step four: and (3) spray granulation, namely putting the slurry filtered in the step three into a spray drying granulation tower, spraying the material into a mist shape through the spray drying granulation tower, and quickly evaporating and drying to obtain the carbon nano tube master batch.
2. The method according to claim 1, wherein in the first and second steps, the carbon nanotube powder, the solvent, the dispersing aid, the lubricant, and the plasticizer are prepared in the following mass parts: 10-15: 25-35, 5-10: 1-10: 10 to 15;
and in the fourth step, the raw materials are heated to 100-130 ℃, spray granulation is carried out in a drying chamber with the spray pressure of 0.1-0.5 Mpa at 120-220 ℃, and the hot air temperature is 120-220 ℃.
3. The preparation equipment for the carbon nanotube master batches is characterized by comprising a granulation tower (1), a heating device and a material returning device (7), wherein the heating device is arranged on one side of the granulation tower (1), the heating device comprises a heater (2), an air blower (21) and a heating pipe (22), an air outlet of the air blower is connected with the heater (2), an air outlet of the heater (2) is connected with the heating pipe (22), one end of the heating pipe (22) enters the center of the top end of an inner cavity of the granulation tower (1) and is provided with a first air injection pipe orifice (222), one side of the heating pipe (22) is provided with a branch pipe (221), one end of the branch pipe (221) horizontally penetrates through the granulation tower (1) and is provided with a second air injection port, and the first air injection pipe orifice (222) and the second air injection pipe orifice (223) are arranged in an up-down opposite manner; a feed pipe (3) is arranged at the top end of the granulation tower (1), one end of the feed pipe (3) longitudinally penetrates through the first air injection pipe opening (222), and a nozzle (31) is arranged in the first air injection pipe opening (222);
a discharge hole (11) is formed in the bottom of the granulation tower (1), a coarse screen component (4), a fine screen component (5) and a driving component (6) for driving the coarse screen component (4) and the fine screen component (5) are arranged in an inner cavity of the granulation tower (1), the coarse screen component (4) comprises a coarse screen plate (41) and a stirring impeller (42), the coarse screen plate (41) is horizontally arranged in the granulation tower (1), a plurality of coarse screen holes (411) are formed in the coarse screen plate (41), and the stirring impeller (42) is rotatably arranged in the center of the sieving plate; the fine screen component (5) is located below the coarse screen component (4), the fine screen component (5) comprises a screen hopper (51), a vibrating motor (52) and a scraping frame (53), the upper end side wall of the screen hopper (51) is connected with the inner wall of the granulation tower (1) through a plurality of elastic supports (54), the bottom of the screen hopper (51) is arranged and installed on an inclined plane, the vibrating motor (52) is arranged on the vibrating plane, one end of the bottom of the screen hopper (51) is obliquely provided with a material conveying pipe (511), the material conveying pipe (511) penetrates through the granulation tower (1) and is connected with a material returning device (7), the material returning device (7) is used for re-conveying particles with smaller size to the granulation tower (1), the middle part of the screen hopper (51) is horizontally provided with a fine screen plate (512), the fine screen plate (512) is provided with a plurality of fine screen holes (5121), the screen hopper (51) is located at the edge of the side wall of the fine screen plate (512) and is circumferentially provided with a plurality of discharge holes (513), the scraping frame (53) is arranged on the fine sieve plate (512), the scraping frame (53) comprises a fixed seat (531) and a plurality of scraping rods (532) which are uniformly distributed on the side wall of the fixed seat (531), the scraping rods (532) are all arranged in an arc structure, one end of each scraping rod (532) extends to the inner wall of the sieving hopper (51), and the bottom of each scraping rod (532) is provided with a soft rubber scraper (5321); drive assembly (6) are located between coarse screen subassembly (4) and fine screen subassembly (5), and drive assembly (6) include gear box (61), transmission shaft (62), driving motor (63), gear box (61) set up at prilling tower (1) inner chamber center, through a plurality of bracing pieces (611) and prilling tower (1) inner wall fixed connection on the lateral wall of gear box (61) upper end, and gear box (61) are improved level and are run through the setting transmission shaft (62), transmission shaft (62) both ends are connected with prilling tower (1) inner wall rotation, and transmission shaft (62) one end is connected with driving motor (63) output, and driving motor (63) set up on prilling tower (1) outer wall and drive transmission shaft (62) rotation, transmission shaft (62) drive stirring impeller (42) and scrape work or material rest (53) rotation through the gear cooperation.
4. The carbon nanotube master batch preparation equipment as claimed in claim 3, wherein the feed back device (7) comprises a feed back pipe (71), a three-way solenoid valve (72), a suction and discharge material cylinder (73), a rotating motor (74) and a lifting assembly, the feed back pipe (71) is longitudinally arranged on one side of the granulation tower (1), the three-way solenoid valve (72) is arranged on the feed back pipe (71), one end of the three-way solenoid valve (72) is connected with the feed back pipe (511), the top end of the feed back pipe (71) is bent and enters the inner cavity of the granulation tower (1), the bottom end of the feed back pipe (71) is connected with the top end of the suction and discharge material cylinder (73), a telescopic air bag (731) is arranged at the upper end of the inner cavity of the suction and discharge material cylinder (73), the center of the top end of the telescopic air bag (731) is arranged in an opening manner, the bottom end of the telescopic air bag (731) is provided with a lifting seat (732), and the rotating motor (74) is arranged on the side wall of the suction and discharge material cylinder (73), and the rotating motor (74) drives the lifting seat (732) to lift through the lifting component and compress the telescopic air bag (731), so that the particles accumulated at the lower end of the material return pipe (71) are blown into the granulation tower (1) again.
5. The carbon nanotube master batch preparation device as claimed in claim 4, wherein a filter screen (711) is arranged in the inner cavity at the lower end of the feed back pipe (71).
6. The apparatus for preparing carbon nanotube master batch according to claim 4, wherein the lifting assembly comprises a rotating disk (75), a linkage rod (76) and a hinge seat (77), the rotating disk (75) is arranged longitudinally, the center of the rotating disk (75) is fixedly connected with the output shaft of the rotating motor (74), two ends of the rotating seat are symmetrically provided with protruding seats (751), one of the protruding seats (751) is vertically provided with a fixed shaft (7511), the fixed seat (531) is provided with one end of the linkage rod (76), the other end of the linkage rod (76) is hinged with the hinge seat (77), and the hinge seat (77) is fixedly arranged at the bottom of the lifting seat (732).
7. The carbon nanotube master batch preparation equipment as claimed in claim 6, wherein a controller (78) and a travel switch (79) are further arranged at the lower end of the inner cavity of the suction and discharge material cylinder (73), the controller (78) is electrically connected with the travel switch (79) and the three-way solenoid valve (72), and contacts of the travel switch (79) are respectively contacted with the protruding seats (751) at the two ends of the rotating seat, so that the contacts of the travel switch (79) are sequentially pressed through the two protruding seats (751) when the rotating seat rotates.
8. The apparatus for preparing carbon nanotube master batch according to claim 3, wherein the stirring impeller (42) comprises a rotating shaft (421) and a plurality of stirring blades (422) uniformly distributed on the rotating shaft (421), and the stirring blades (422) are all curved in an arc shape.
9. The apparatus for preparing carbon nanotube master batch as claimed in claim 3, wherein the fine screen plate (512) is disposed with its peripheral edge inclined upward, and the end of the scraping bar (532) is also bent upward and adapted to the fine screen plate (512).
10. The preparation equipment of the carbon nanotube master batch according to claim 3, wherein the transmission shaft (62) is provided with a first bevel gear (621), the upper end and the lower end of the first bevel gear (621) are respectively engaged with a second bevel gear (641) and a third bevel gear (651), the second bevel gear (641) and the third bevel gear (651) are respectively arranged on the upper connecting shaft (64) and the lower connecting shaft (65), the upper connecting shaft (64) and the lower connecting shaft (65) are respectively rotatably arranged on the upper end and the lower end of the gear box (61), and the upper connecting shaft (64) and the lower connecting shaft (65) are respectively connected with the rotating shaft (421) and the fixing seat (531).
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