CN114053937A - Preparation method and device of graphene mixed powder - Google Patents

Preparation method and device of graphene mixed powder Download PDF

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Publication number
CN114053937A
CN114053937A CN202111413782.8A CN202111413782A CN114053937A CN 114053937 A CN114053937 A CN 114053937A CN 202111413782 A CN202111413782 A CN 202111413782A CN 114053937 A CN114053937 A CN 114053937A
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bin
graphene
mixing
grinding
filter plate
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CN202111413782.8A
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CN114053937B (en
Inventor
王炜
王登诗
巫伟伟
举亚琪
刘双翼
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Chongqing Institute Of Graphene
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Chongqing Institute Of Graphene
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B02CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
    • B02CCRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
    • B02C17/00Disintegrating by tumbling mills, i.e. mills having a container charged with the material to be disintegrated with or without special disintegrating members such as pebbles or balls
    • B02C17/10Disintegrating by tumbling mills, i.e. mills having a container charged with the material to be disintegrated with or without special disintegrating members such as pebbles or balls with one or a few disintegrating members arranged in the container
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B02CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
    • B02CCRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
    • B02C17/00Disintegrating by tumbling mills, i.e. mills having a container charged with the material to be disintegrated with or without special disintegrating members such as pebbles or balls
    • B02C17/18Details
    • B02C17/183Feeding or discharging devices
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B02CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
    • B02CCRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
    • B02C17/00Disintegrating by tumbling mills, i.e. mills having a container charged with the material to be disintegrated with or without special disintegrating members such as pebbles or balls
    • B02C17/18Details
    • B02C17/20Disintegrating members
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B02CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
    • B02CCRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
    • B02C19/00Other disintegrating devices or methods
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B02CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
    • B02CCRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
    • B02C19/00Other disintegrating devices or methods
    • B02C19/18Use of auxiliary physical effects, e.g. ultrasonics, irradiation, for disintegrating
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B02CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
    • B02CCRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
    • B02C21/00Disintegrating plant with or without drying of the material
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B02CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
    • B02CCRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
    • B02C23/00Auxiliary methods or auxiliary devices or accessories specially adapted for crushing or disintegrating not provided for in preceding groups or not specially adapted to apparatus covered by a single preceding group
    • B02C23/02Feeding devices
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B02CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
    • B02CCRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
    • B02C23/00Auxiliary methods or auxiliary devices or accessories specially adapted for crushing or disintegrating not provided for in preceding groups or not specially adapted to apparatus covered by a single preceding group
    • B02C23/08Separating or sorting of material, associated with crushing or disintegrating
    • B02C23/16Separating or sorting of material, associated with crushing or disintegrating with separator defining termination of crushing or disintegrating zone, e.g. screen denying egress of oversize material

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  • Engineering & Computer Science (AREA)
  • Food Science & Technology (AREA)
  • Health & Medical Sciences (AREA)
  • Toxicology (AREA)
  • Carbon And Carbon Compounds (AREA)

Abstract

The invention relates to the field of graphene, and discloses a preparation method of graphene mixed powder, which comprises extruding graphene powder from a filter plate in a grinding mode, and mixing the graphene powder with a spray-shaped auxiliary material; the device comprises a feed inlet, a spiral propelling bin, a grinding bin, a filter plate, a mixing bin and a discharge outlet from top to bottom in sequence, wherein a spiral propeller is arranged in the spiral propelling bin, a ball milling medium is filled in the spiral propelling bin, and the spiral propelling bin is also connected with an ultrasonic generator; a spherical grinding head is arranged in the grinding bin, the tail of the spherical grinding head is connected with the spiral propeller, and the head of the spherical grinding head is contacted with the filter plate; the filter plate is arranged between the grinding bin and the mixing bin, and the mixing bin is provided with a spraying device. The invention aims to solve the problem of uneven mixing of graphene and other raw materials, and provides a method and a device for preparing graphene mixed powder with more uniform mixing.

Description

Preparation method and device of graphene mixed powder
Technical Field
The invention relates to the field of graphene, and particularly relates to a preparation method and a preparation device of graphene mixed powder.
Background
Graphene (Graphene) is a new material with sp hybridized connected carbon atoms tightly packed into a single-layer two-dimensional honeycomb lattice structure. The graphene has excellent optical, electrical and mechanical properties, has important application prospects in the aspects of materials science, micro-nano processing, energy, biomedicine, drug delivery and the like, and is considered to be a revolutionary material in the future.
Graphene is usually mixed with various raw materials due to excellent performance, and the graphene is mixed with various materials including a catalyst, a conductive agent, an initiator and the like and applied in various fields, but when the graphene is stirred and mixed with other raw materials, due to the characteristic that the graphene is easy to agglomerate, the mixing difficulty is high, and when the components are more, the graphene needs to be added one by one, which is very troublesome, and the graphene has an adsorption effect on the materials such as the catalyst, the adhesive and the like, so that the mixing difficulty is higher, once the graphene cannot be uniformly mixed, the performance of the materials can be greatly influenced, for example, when an electrode material is manufactured, the adhesive, the catalyst and the conductive agent need to be added, and if the graphene cannot be uniformly mixed with the raw materials, the balance of the electrode is greatly influenced, the internal resistance is increased, and the electrode performance is reduced.
Disclosure of Invention
The invention aims to solve the problem of uneven mixing of graphene and other raw materials, and provides a method and a device for preparing graphene mixed powder with more uniform mixing.
The basic technical scheme of the invention is as follows: the preparation method of the graphene mixed powder comprises the steps of extruding graphene powder from a filter plate in a grinding mode, and mixing the graphene powder with a spray-shaped auxiliary material.
Grinding accelerates dispersion of graphene on one hand and reduces agglomeration of graphene on the other hand; the graphene powder is extruded from the filter plate in a grinding mode, the graphene is extruded from the filter holes of the filter plate by the extrusion force generated by grinding, and when the graphene is extruded, the graphene is dispersed, and then is mixed with other sprayed auxiliary materials instantly; other auxiliary materials can be mixed uniformly in advance, and one type of auxiliary material can be sprayed and mixed with graphene powder simultaneously, so that compared with a mechanical mixing mode, the mixing uniformity is improved.
Further, the graphene powder is fed by a screw propulsion mode with a ball milling medium before grinding. Ball milling and spiral propelling act simultaneously, so that graphene powder can be further dispersed by ball milling, and graphene powder can be propelled to a process needing to be ground.
Further, the operation of spirally propelling the graphene powder with the ball milling medium is performed in an ultrasonic environment. The ultrasonic assistance is assisted, and the ultrasonic is added with ball milling, so that the dispersion is more uniform.
Further, the graphene powder is nanoscale graphene powder.
Furthermore, the filter plate is made of elastic materials, and the diameter of the filter holes is nanometer and micron. When the filter plate is not ground, graphene powder hardly penetrates through the filter plate, and the graphene powder can be extruded from the filter holes only when being ground and extruded.
Further, the filter plate adopts high strength filter cloth, and the breaking strength of filter cloth is: warp direction > 6000N/5X 20cm, weft direction > 4000N/5X 20cm, elongation at break < 5%. Compared with a hard filter plate, the filter cloth made of the elastic material is thin in cloth thickness, so that the possibility of graphene agglomeration in holes can be reduced, and the high-strength filter cloth is not easy to damage during grinding.
According to another technical scheme provided by the invention, the preparation device of the graphene mixed powder sequentially comprises a feeding hole, a spiral propelling bin, a grinding bin, a filter plate, a mixing bin and a discharging hole from top to bottom, wherein a spiral propeller is arranged in the spiral propelling bin, a ball milling medium is filled in the spiral propelling bin, and the spiral propelling bin is also connected with an ultrasonic generator; a spherical grinding head is arranged in the grinding bin, the tail of the spherical grinding head is connected with the spiral propeller, and the head of the spherical grinding head is contacted with the filter plate; the filter plate is arranged between the grinding bin and the mixing bin, and the mixing bin is provided with a spraying device.
The preparation device of the graphene mixed powder can realize the preparation method of the graphene, in the device, a spiral propeller in a spiral propelling bin is externally connected with a power motor to rotate, blades of the spiral propeller are close to the bin wall of a grinding bin, a ball milling medium is filled between the blades of the spiral propeller in the grinding bin and the bin wall, the ball milling medium rolls while propelling to realize ball milling of the graphene powder, an ultrasonic generator provides ultrasonic mechanical waves, and the ultrasonic waves are utilized to accelerate the dispersion of the graphene powder while ball milling and propelling; the grinding in the grinding bin adopts a spherical grinding head, the power of the spherical grinding head comes from a screw propeller, the head of the spherical grinding head is in contact with the filter plate, the head is ground by friction with the filter plate, and the ground graphene powder can leak out of the filter holes of the filter plate, so that the graphene powder is dispersed; the spraying device is used for spraying the auxiliary materials in a spraying manner, the powdery materials are sprayed, the liquid materials are sprayed in a mist manner, and the mist or powdery auxiliary materials are contacted and adsorbed with the dispersed graphene powder so as to be uniformly mixed.
Furthermore, the filter plate adopts high-strength filter cloth which is detachably connected with the bin walls of the grinding bin and the mixing bin respectively. The connecting parts of the high-strength filter cloth, the grinding bin and the mixing bin can be provided with extension ears which are connected by bolts.
Further, the ultrasonic generator is connected with the screw propeller. Compare supersonic generator and the bulkhead connection in spiral propulsion storehouse, be connected with screw propeller, along with screw propeller's rotation, the wave reach of ultrasonic wave is wider, and dispersion effect is better.
Furthermore, the spray heads of the spraying device are arranged in a plurality of numbers, the spray heads are evenly embedded on the wall of the mixing material bin in the same circumferential direction, and the number and the density of the spray heads on the upper portion of the mixing material bin are larger than those of the spray heads on the lower portion of the mixing material bin. When oozing from the filter plate at graphite alkene powder, graphite alkene powder's dispersibility is highest this moment, most auxiliary materials attach to the surface of graphite alkene powder simultaneously at this moment, and along with graphite alkene powder village whereabouts, when its adsorption agglomeration can increase gradually, most auxiliary materials have mixed the even with graphite alkene powder, consequently, the shower nozzle quantity and the density of blending bunker are greater than shower nozzle quantity and the density of blending bunker lower part, guarantee along with graphite alkene powder's whereabouts, the injected volume of auxiliary material reduces gradually, graphite alkene powder is higher with the homogeneity of mixing of auxiliary material.
Drawings
Fig. 1 is a schematic view of a graphene mixed powder preparation apparatus according to the present invention;
fig. 2 is a longitudinal sectional view of fig. 1.
Detailed Description
The following is further detailed by way of specific embodiments:
reference numerals in the drawings of the specification include: the device comprises a feed inlet 1, a spiral propelling bin 2, a grinding bin 3, a filter plate 4, a mixing bin 5, a discharge port 6, a spiral propeller 7, a ball milling medium 8, a spherical grinding head 9 and a spray head 10.
The first embodiment is as follows: the invention relates to a preparation device of graphene mixed powder, which is shown in the attached drawings 1 and 2:
the device for preparing the graphene mixed powder sequentially comprises a feed inlet 1, a spiral propelling bin 2, a grinding bin 3, a filter plate 4, a mixing bin 5 and a discharge port 6 from top to bottom, wherein the feed inlet 1 is a funnel and is communicated with the spiral propelling bin 2, the diameter of the spiral propelling bin 2 is 30cm or can be 30-50cm, a spiral propeller 7 is arranged in the spiral propelling bin, the spiral propeller 7 comprises a screw rod and a rotating blade welded on the screw rod, a ball milling medium 8 is filled between the rotating blade and the bin wall of the spiral propelling bin 2, the ball milling medium 88 adopts stainless steel balls, the spiral propeller 7 is also connected with an ultrasonic generator (not shown in the figure), and the ultrasonic generator adopts a high-power ultrasonic generator with the ultrasonic power of 3000W and the frequency of 40 KHZ; the joints of the spiral propelling bin 2 and the grinding bin 3 are provided with connecting lugs for connection (namely, the joints of the spiral propelling bin and the grinding bin extend outwards for a circle, and refer to the connection of a chemical reaction kettle in the prior art), the connecting lugs are connected by bolts, the tail part of a spherical grinding head 9 in the grinding bin 3 is welded with a spiral propeller 7, and the head part of the spherical grinding head 9 is contacted with a filter plate 4; the filter plate 4 adopts high-strength filter cloth, and the breaking strength of the filter cloth is as follows: the warp direction is more than 6000N/5 x 20cm, the weft direction is more than 4000N/5 x 20cm, the elongation at break is less than 5%, the aperture of the filter cloth is nano-scale or micron-scale, the aperture of the filter cloth is between 5 microns and 100 microns (refer to high-strength high-modulus polyethylene composite fiber filter cloth produced by Shandong Aidi Polymer materials Co., Ltd., PCT patent application No. WO2015021570A 1), the connecting lugs are extended at the connecting parts of the high-strength filter cloth, the grinding bin 3 and the bin wall of the mixing bin 5, the connecting lugs are detachably connected through bolts, the mixing bin 5 is connected with a spraying device, the bin wall of the mixing bin 5 is provided with a plurality of threaded holes, the spraying heads 10 of the spraying device are in threaded connection in the threaded holes, the plurality of spraying heads 10 are uniformly arranged on the same circumference direction on the bin wall of the mixing bin 5, and the number and density of the spraying heads 10 at the upper part of the mixing bin 5 are larger than the number and density of the spraying heads 10 at the lower part of the mixing bin 5, the discharge port 6 is in an inverted funnel shape and is communicated with the bottom of the mixing bin 5.
In specific implementation, 50kg of nano-scale graphene powder is poured from the feeding hole 1 and enters the spiral propelling bin 2, and under the ultrasonic vibration of the ultrasonic generator, the nano-scale graphene powder flows to the spiral propelling bin along with the rotation of the spiral propeller 7Advancing, entering the ball milling media 8 of the stainless steel balls, grinding and dispersing while advancing, and dispersing the nano graphene powder by ultrasonic assistance; the nano graphene powder enters a grinding bin 3 after being pushed, and falls on a filter plate 4 after entering the grinding bin 3, namely falls on high-density filter cloth, the spherical grinding head 9 rotates on the filter cloth under the drive of a spiral propeller 7, the nano graphene powder on the filter cloth is ground and dispersed again by the spherical grinding head 9, the dispersed nano graphene powder leaks out of the aperture of the filter cloth and falls into a mixing bin while being ground and extruded, a spray head 10 in threaded connection on the wall of the mixing bin 5 is externally connected with a pressurized storage bin, and auxiliary materials comprise 1kg of allyl polyoxyethylene polyoxypropylene ether, 8kg of N-allyl imidazole, 3kg of hydrogen peroxide, 3kg of tert-butyl peroxybenzoate, 3kg of Al2O32kg of silver paste, 6kg of silver paste and 4kg of polyacrylate; firstly, the auxiliary materials are stirred and mixed uniformly in another mixer, the mixture is added into a storage bin, a connecting pipe of the storage bin is connected with a plurality of spray heads 10, the spray heads 10 spray the vaporific auxiliary material mixture, the vaporific auxiliary material mixture is uniformly mixed with the dispersed nano graphene powder leaked from the filter cloth, and the graphene mixed powder is obtained by discharging from a discharge port 6.
The foregoing is merely an example of the present invention and common general knowledge of known specific structures and features of the embodiments is not described herein in any greater detail. It should be noted that variations and modifications can be made by those skilled in the art without departing from the structure of the present invention. These should also be construed as the scope of the present invention, and they should not be construed as affecting the effectiveness of the practice of the present invention or the applicability of the patent. The scope of the claims of the present application shall be determined by the contents of the claims, and the description of the embodiments and the like in the specification shall be used to explain the contents of the claims.

Claims (10)

1. The preparation method of the graphene mixed powder is characterized by comprising the following steps: extruding the graphene powder from the filter plate in a grinding mode, and mixing the graphene powder with a spray-shaped auxiliary material.
2. The method for preparing the graphene mixed powder according to claim 1, wherein the method comprises the following steps: the graphene powder is fed in a spiral propelling mode with a ball milling medium before grinding.
3. The method for preparing the graphene mixed powder according to claim 2, wherein: the operation of the spiral propelling graphene powder with the ball milling medium is carried out in an ultrasonic environment.
4. The method for preparing the graphene mixed powder according to any one of claims 1 to 3, wherein: the graphene powder is nano-grade graphene powder.
5. The method for preparing the graphene mixed powder according to claim 4, wherein: the filter plate is made of elastic material, and the diameter of the filter holes is nanometer and micron.
6. The method for preparing the graphene mixed powder according to claim 5, wherein: the filter plate adopts high-strength filter cloth, and the breaking strength of the filter cloth is as follows: warp direction > 6000N/5X 20cm, weft direction > 4000N/5X 20cm, elongation at break < 5%.
7. A preparation facilities for the mixed powder of graphite alkene of claim 4, characterized by: the ball milling device sequentially comprises a feed inlet, a spiral propelling bin, a grinding bin, a filter plate, a mixing bin and a discharge outlet from top to bottom, wherein a spiral propeller is arranged in the spiral propelling bin, a ball milling medium is filled in the spiral propelling bin, and the spiral propelling bin is also connected with an ultrasonic generator; a spherical grinding head is arranged in the grinding bin, the tail of the spherical grinding head is connected with the spiral propeller, and the head of the spherical grinding head is contacted with the filter plate; the filter plate is arranged between the grinding bin and the mixing bin, and the mixing bin is connected with a spraying device.
8. The apparatus for preparing graphene mixed powder according to claim 7, wherein: the filter plate adopts high-strength filter cloth which is detachably connected with the bin walls of the grinding bin and the mixing bin respectively.
9. The apparatus for preparing graphene mixed powder according to claim 8, wherein: the ultrasonic generator is connected with the spiral propeller.
10. The apparatus for preparing graphene mixed powder according to claim 9, wherein: the spray heads of the spraying device are provided with a plurality of spray heads which are evenly embedded on the wall of the mixing material bin in the same circumferential direction, and the number and the density of the spray heads on the upper part of the mixing material bin are greater than those of the spray heads on the lower part of the mixing material bin.
CN202111413782.8A 2021-11-25 2021-11-25 Preparation method and device of graphene mixed powder Active CN114053937B (en)

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Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4577805A (en) * 1984-05-31 1986-03-25 Sperry Corporation Agricultural mixing and grinding machine
CN104629495A (en) * 2015-02-15 2015-05-20 江苏金陵特种涂料有限公司 Preparation method for graphene
CN110369087A (en) * 2019-06-05 2019-10-25 福建创源石墨烯科技有限公司 A kind of apparatus for grinding and dispersing of grapheme material
CN210419252U (en) * 2019-06-23 2020-04-28 奇华光电(昆山)股份有限公司 Device for preparing graphene powder
CN212791239U (en) * 2020-07-10 2021-03-26 金华市美林涂料有限公司 Horizontal sand mill with internal circulation
CN113185855A (en) * 2021-04-19 2021-07-30 长沙天源羲王材料科技有限公司 Preparation method and automation equipment of graphene modified powder
CN213914040U (en) * 2020-11-05 2021-08-10 福建智维石墨烯科技有限公司 Raw material grinding device for processing graphene paint

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4577805A (en) * 1984-05-31 1986-03-25 Sperry Corporation Agricultural mixing and grinding machine
CN104629495A (en) * 2015-02-15 2015-05-20 江苏金陵特种涂料有限公司 Preparation method for graphene
CN110369087A (en) * 2019-06-05 2019-10-25 福建创源石墨烯科技有限公司 A kind of apparatus for grinding and dispersing of grapheme material
CN210419252U (en) * 2019-06-23 2020-04-28 奇华光电(昆山)股份有限公司 Device for preparing graphene powder
CN212791239U (en) * 2020-07-10 2021-03-26 金华市美林涂料有限公司 Horizontal sand mill with internal circulation
CN213914040U (en) * 2020-11-05 2021-08-10 福建智维石墨烯科技有限公司 Raw material grinding device for processing graphene paint
CN113185855A (en) * 2021-04-19 2021-07-30 长沙天源羲王材料科技有限公司 Preparation method and automation equipment of graphene modified powder

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