CN112481644A - Flower-shaped graphene, melt-blown fabric, preparation method of flower-shaped graphene and melt-blown fabric, and mask - Google Patents
Flower-shaped graphene, melt-blown fabric, preparation method of flower-shaped graphene and melt-blown fabric, and mask Download PDFInfo
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 128
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 96
- 239000004744 fabric Substances 0.000 title claims abstract description 40
- 238000002360 preparation method Methods 0.000 title abstract description 12
- 239000002131 composite material Substances 0.000 claims abstract description 24
- 239000000463 material Substances 0.000 claims abstract description 24
- 238000001914 filtration Methods 0.000 claims abstract description 14
- 238000011282 treatment Methods 0.000 claims abstract description 8
- 239000002086 nanomaterial Substances 0.000 claims abstract description 7
- 239000010410 layer Substances 0.000 claims abstract description 5
- 239000002356 single layer Substances 0.000 claims abstract description 3
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 44
- 229910002804 graphite Inorganic materials 0.000 claims description 38
- 239000010439 graphite Substances 0.000 claims description 38
- -1 polypropylene Polymers 0.000 claims description 25
- 239000003792 electrolyte Substances 0.000 claims description 23
- 239000004743 Polypropylene Substances 0.000 claims description 22
- 239000000835 fiber Substances 0.000 claims description 22
- 229910052697 platinum Inorganic materials 0.000 claims description 22
- 229920001155 polypropylene Polymers 0.000 claims description 22
- 238000001035 drying Methods 0.000 claims description 19
- 239000011347 resin Substances 0.000 claims description 19
- 229920005989 resin Polymers 0.000 claims description 19
- 239000004594 Masterbatch (MB) Substances 0.000 claims description 16
- 238000007664 blowing Methods 0.000 claims description 16
- 239000000155 melt Substances 0.000 claims description 16
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B1/00—Electrolytic production of inorganic compounds or non-metals
-
- A—HUMAN NECESSITIES
- A41—WEARING APPAREL
- A41D—OUTERWEAR; PROTECTIVE GARMENTS; ACCESSORIES
- A41D13/00—Professional, industrial or sporting protective garments, e.g. surgeons' gowns or garments protecting against blows or punches
- A41D13/05—Professional, industrial or sporting protective garments, e.g. surgeons' gowns or garments protecting against blows or punches protecting only a particular body part
- A41D13/11—Protective face masks, e.g. for surgical use, or for use in foul atmospheres
-
- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
- D04H1/54—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties by welding together the fibres, e.g. by partially melting or dissolving
- D04H1/56—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties by welding together the fibres, e.g. by partially melting or dissolving in association with fibre formation, e.g. immediately following extrusion of staple fibres
Abstract
The invention belongs to the field of graphene preparation and application, and particularly relates to flower-shaped graphene based on electrochemical treatment, a preparation method of the flower-shaped graphene and application of the flower-shaped graphene in melt-blown products. The flower-like graphene is composed of a plurality of independent graphene aggregates, wherein the graphene aggregates are formed by curling single-layer or multi-layer ultrathin two-dimensional nano materials, and the size of each single graphene aggregate is 50-200 nm. The flower-like graphene material can effectively improve the air permeability of the filtering performance of the composite melt-blown fabric, and endows the composite melt-blown fabric with excellent antibacterial performance and mechanical performance. The melt-blown fabric prepared from the flower-like graphene has excellent performances of oleophylic and hydrophobic property, antibacterial and bacteriostatic properties, strong adsorption capacity and the like, and the prepared mask has a great practical application value in resisting epidemic situations.
Description
Technical Field
The invention belongs to the field of graphene preparation and application, and particularly relates to flower-shaped graphene based on electrochemical treatment, a preparation method of the flower-shaped graphene and application of the flower-shaped graphene in melt-blown products.
Background
The melt-blown cloth is formed by disordered accumulation of micron-sized fibers, extremely fine particles are formed and filtered into narrow gaps and detention spaces, and after electret treatment, electrostatic charges loaded on the fibers can capture the fine particles through coulomb force, so that the manufactured mask is suitable in breathing resistance and comfortable to wear. Since new crown epidemic outbreak in 2020, the mask becomes a necessary article for people to live, work and go out, and people also put forward higher requirements on the filtering performance, the air permeability, the service life and even the antibacterial effect of the mask.
Graphene is an ultrathin two-dimensional nano material with the thickness of only 0.34nm, has outstanding excellent chemical stability and mechanical property, super-strong heat conduction performance and electric conductivity, and also has strong ion exchange performance and adsorption performance, and can be widely applied to the fields of air purification, water treatment, energy storage, catalysis and the like. Similarly, graphene can also play an important role in meltblown fabrics and masks. The graphene nanosheets are assembled into a certain three-dimensional structure and uniformly dispersed into the melt-blown cloth, so that the advantage of large specific surface area can be exerted, and particles in air can be fully adsorbed, so that the air permeability is greatly improved while the filtering performance is kept.
In the related preparation technologies of the graphene/polypropylene composite master batch and the melt-blown fabric thereof, for example, CN202010580101.6 discloses a graphene composite melt-blown fabric with high filtering performance and a preparation method thereof, although the graphene melt-blown fabric is also described, the graphene melt-blown fabric is only limited to introduce components of the melt-blown fabric, and the influence of the structural characteristics of graphene on the melt-blown fabric performance is not deeply researched by using a graphene material. Meanwhile, in order to meet the requirement of uniformity of the product, a large amount of various additives and additives are used, so that the performance of the product is reduced due to the residues of the various additives and additives in the product. For example, in the existing graphene/polypropylene composite master batch, the mass fraction of the auxiliary agent is as high as 1-5%, which affects the processing performance of the graphene/polypropylene composite master batch to a certain extent and causes the quality of a melt-blown fabric product to be reduced and the performance to be reduced.
Disclosure of Invention
The purpose of the invention is as follows: the flower-shaped graphene is controllable in structure, oleophylic, hydrophobic, antibacterial, bacteriostatic and strong in adsorption capacity, and the melt-blown cloth and the mask adopting the graphene are provided.
In addition, the invention also provides a preparation method of the flower-shaped graphene and the melt-blown fabric.
The technical scheme of the invention is as follows: the utility model provides a flower form graphite alkene, comprises a plurality of mutually independent graphite alkene aggregates, wherein the graphite alkene aggregate is curled by monolayer or the ultra-thin two-dimensional nano-material of multilayer and forms, single graphite alkene aggregate size is between 50 ~ 200nm, and the structure is even stable, and can effectively keep the independence of each aggregate and not take place the secondary and reunite to improve external contact area.
The graphene aggregate single structural body is arranged in the center of a scroll, and is coiled into a flower-shaped structure by a belt-shaped ultrathin two-dimensional nano material around the center of the scroll.
The number of the curled layers of the graphene aggregate is 2-20, so that the specific adsorption performance and sterilization performance of graphene can be effectively exerted.
A preparation method of the flower-like graphene comprises the following steps:
(1) a graphite rod is used as an anode, and a metal electrode is used as a cathode;
(2) configuration of KOH/H2O2The aqueous solution is used as electrolyte;
(3) the graphite rod and the metal electrode are used as electrodes of an electrolytic cell and are placed in the electrolytic cell, the electrode position is adjusted, the graphite rod and the metal electrode are immersed in electrolyte, the graphite rod and the metal electrode are connected with a direct current power supply by using a lead, the anode is connected with the anode of the direct current power supply, the cathode is connected with the cathode of the direct current power supply, and after the direct current power supply applies direct current voltage, an electrolytic reaction is carried out;
(4) in the electrolysis process, bubbles are continuously generated on the anode graphite rod, and the color of the electrolyte is changed from colorless to black;
(5) after the electrolysis is finished, filtering the electrolyte to obtain a black product, and cleaning the black product by using distilled water;
(6) and drying the cleaned black powder to obtain the flower-like graphene.
The concentration of KOH in the step (2) is0.1M～10M，H2O2The concentration of the graphene is 10 mM-1M, so that a proper reaction speed is achieved, the stable and consistent structure of the flower-shaped graphene can be ensured, and the yield is stable.
In the step (3), the purity of the graphite rod is not lower than 99.9%, excessive impurity components in the flower-shaped graphene are prevented, the filtering or antibacterial performance is reduced, and the performance requirements or chemical component requirements of the final product cannot be met. The metal anode adopts a platinum electrode, and the distance between the cathode and the anode is 3-10 cm, so that the unstable structure of the flower-shaped graphene due to insufficient electrolysis is avoided.
And (3) in the step (3), the direct-current voltage is 0.1-20V, the temperature of an electrolytic reaction system is not higher than 50 ℃, and the stripping reaction caused by overhigh temperature is prevented from being accelerated, so that the structure of the flower-shaped graphene material is unstable.
The melt-blown fabric comprises melt-blown fibers containing the flower-like graphene, the mass content of the flower-like graphene in the melt-blown fibers is 0.001% -1%, the phenomenon of uneven dispersion caused by overhigh content is avoided, and evidence shows that the beneficial synergy of the excessively high content of the flower-like graphene on a melt-blown fabric product is very limited.
A method of making the meltblown fabric according to the invention by:
(1) preparing the composite master batch: respectively weighing a certain amount of flower-like graphene, a dispersing agent and a polypropylene resin material, uniformly mixing and stirring the three raw materials, adding the mixture into a double-screw extruder, setting the temperature of each interval of the extruder, starting the extruder to extrude strands, and then cooling, granulating and drying to obtain the composite master batch;
(2) and (3) melt-blown process treatment: taking a certain amount of the composite master batch prepared in the step (1) and a certain amount of polypropylene resin material, uniformly mixing the two materials, sending the mixture into melt-blowing equipment for melt-blowing spinning, spraying a melt from a screw to a spinning assembly to a spinneret plate, and drawing the melt by high-temperature high-speed airflow to prepare melt-blown superfine fiber;
(3) performing electret treatment: and (3) winding the melt-blown superfine fibers prepared in the step (2), performing electrostatic electret, slitting and winding to obtain the melt-blown product with flower-like graphene as the filler.
In the step (1), the mass ratio of the flower-shaped graphene to the dispersing agent to the polypropylene resin material is 0.01-10: 0.1-1: 99.89-89; in the step 1, the extrusion temperature is 150-250 ℃.
The mass ratio of the composite master batch to the polypropylene resin material in the step (2) is 0.1-10: 99.9-90; in the step (2), the extrusion temperature is 160-280 ℃, and the receiving distance is 7-25 cm.
A mask adopts the melt-blown fabric.
The invention has the beneficial effects that: the flower-shaped graphene prepared by the invention has a large number of curled aggregate structures inside, so that the graphene has low surface functional group content, is high in hydrophobicity, and can effectively avoid molecular aggregation in a respiration process; graphene can also generate reactive oxygen species, thereby inducing oxidative stress, causing disruption of microbial activity by oxidizing cellular structures or components. Therefore, the melt-blown fabric containing the flower-like graphene has the characteristics of high filtering performance, good air permeability, excellent antibacterial and bacteriostatic properties, long service life and the like, and the stretch-resistant performance of the melt-blown fabric added with the graphene is improved, which means that the graphene melt-blown fabric is firmer, and correspondingly, the manufactured mask is firmer and more durable, so the comprehensive performance of the mask is superior to that of the common melt-blown fabric and the conventional graphene melt-blown fabric. In addition, the preparation process of the melt-blown fabric adopting the flower-shaped graphene is simple, mass production can be realized, the cost is low, and the mask manufactured by the method has extremely high practical application value in epidemic situations and even a considerable period of time after the epidemic situations pass.
Drawings
FIG. 1 is an electrolytic schematic diagram of the preparation of flower-like graphene according to the present invention;
fig. 2 is a Transmission Electron Microscope (TEM) picture of flower-like graphene prepared in example 1;
fig. 3 is a Transmission Electron Microscope (TEM) picture of flower-like graphene prepared in example 2.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the following detailed description, but those skilled in the art will understand that the following described examples are some, not all, of the examples of the present invention, and are only used for illustrating the present invention, and should not be construed as limiting the scope of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
Example 1
(1) A high-purity graphite rod is used as an anode, and a platinum electrode is used as a cathode; configuration of KOH/H2O2The electrolyte is an aqueous solution, wherein the concentration of KOH is 5M, and H2O2Is 20 mM.
(2) Referring to fig. 1, a high-purity graphite rod and a platinum electrode are placed in an electrolytic cell, the electrode spacing is adjusted to be 5cm, the graphite rod and the platinum electrode are immersed in electrolyte, the high-purity graphite rod and the platinum electrode are connected with a direct current power supply through a lead, the anode is connected with the anode of the direct current power supply, the cathode is connected with the cathode of the direct current power supply, and after the direct current power supply applies a direct current voltage of 15V, an electrolytic reaction is performed at room temperature; after the electrolysis is finished, filtering the electrolyte to obtain a black product, and cleaning the black product by using distilled water;
(3) drying the cleaned black powder in a drying oven to obtain flower-like graphene, referring to fig. 2, which is a Transmission Electron Microscope (TEM) picture of the flower-like graphene prepared in this embodiment, it can be seen that the prepared graphene is rolled into a rosette shape, and the size is about 100 nm. This flower form graphite alkene is curled by 10 layers and thickness no longer than 1 nm's ultra-thin two-dimensional nano-material and forms, and surface functional group content is less, presents for high hydrophobicity, can effectively avoid the gathering of breathing in-process molecule, and the edge of flower form graphite alkene is comparatively sharp simultaneously, can utilize its sharp edge to cause physical damage to the bacterium, thereby draws out its integrality with the phospholipid in its cell membrane, finally leads to the outflow of cytoplasm, consequently has better antibacterial property.
(4) Weighing flower-shaped graphene, a dispersing agent and a polypropylene resin material according to a mass ratio of 0.01: 0.1:99.89, mixing and stirring uniformly, adding into a double-screw extruder, setting the temperature of each section of the extruder to be 150 ℃, starting the extruder to extrude strand wires, and then cooling, granulating and drying to obtain the composite master batch.
(5) Uniformly mixing the composite master batches and the polypropylene resin material according to the mass ratio of 2:98, feeding the mixture into melt-blowing equipment for melt-blowing spinning, spraying a melt from a screw to a spinning assembly to a spinneret plate, and drawing the melt by high-temperature high-speed airflow to prepare melt-blown superfine fibers;
(6) and (3) winding, electrostatically electret, slitting and rolling the melt-blown superfine fibers to obtain the melt-blown fabric taking flower-shaped graphene as the filler.
Example 2
(1) A high-purity graphite rod is used as an anode, and a platinum electrode is used as a cathode; configuration of KOH/H2O2The electrolyte is an aqueous solution, wherein the concentration of KOH is 5M, and H2O2Is 20 mM.
(2) Putting a high-purity graphite rod and a platinum electrode into an electrolytic cell, adjusting the distance between the electrodes to be 6cm, immersing the graphite rod and the platinum electrode into electrolyte, connecting the high-purity graphite rod and the platinum electrode with a direct-current power supply by using a lead, connecting an anode with the anode of the direct-current power supply, connecting a cathode with the cathode of the direct-current power supply, and carrying out an electrolytic reaction at room temperature after the direct-current power supply applies a direct-current voltage of 15V; after the electrolysis is finished, filtering the electrolyte to obtain a black product, and cleaning the black product by using distilled water;
(3) drying the cleaned black powder in a drying oven to obtain flower-like graphene, referring to fig. 3, which is a Transmission Electron Microscope (TEM) picture of the flower-like graphene prepared in this embodiment, the shape and structure of which are similar to those of embodiment 1, and the size of which is also close to that of embodiment 1, which shows that the product prepared by the method of the present invention has good stability, good manufacturability and good quality.
(4) Weighing flower-shaped graphene, a dispersing agent and a polypropylene resin material according to a mass ratio of 0.01: 0.1:99.89, mixing and stirring uniformly, adding into a double-screw extruder, setting the temperature of each section of the extruder to be 150 ℃, starting the extruder to extrude strand wires, and then cooling, granulating and drying to obtain the composite master batch.
(5) Uniformly mixing the composite master batches and the polypropylene resin material according to the mass ratio of 2:98, feeding the mixture into melt-blowing equipment for melt-blowing spinning, spraying a melt from a screw to a spinning assembly to a spinneret plate, and drawing the melt by high-temperature high-speed airflow to prepare melt-blown superfine fibers;
(6) and (3) winding, electrostatically electret, slitting and rolling the melt-blown superfine fibers to obtain the melt-blown fabric taking flower-shaped graphene as the filler.
Example 3
(1) A high-purity graphite rod is used as an anode, and a platinum electrode is used as a cathode; configuration of KOH/H2O2The electrolyte is aqueous solution, wherein the concentration of KOH is 10M, and H2O2Is 100 mM.
(2) Putting a high-purity graphite rod and a platinum electrode into an electrolytic cell, adjusting the distance between the electrodes to be 5cm, immersing the graphite rod and the platinum electrode into electrolyte, connecting the high-purity graphite rod and the platinum electrode with a direct-current power supply by using a lead, connecting an anode with the anode of the direct-current power supply, connecting a cathode with the cathode of the direct-current power supply, and carrying out an electrolytic reaction at room temperature after the direct-current power supply applies a direct-current voltage of 15V; after the electrolysis is finished, filtering the electrolyte to obtain a black product, and cleaning the black product by using distilled water;
(3) and drying the cleaned black powder in a drying oven to obtain the flower-shaped graphene.
(4) Weighing flower-shaped graphene, a dispersing agent and a polypropylene resin material according to a mass ratio of 0.01: 0.1:99.89, mixing and stirring uniformly, adding into a double-screw extruder, setting the temperature of each section of the extruder to be 150 ℃, starting the extruder to extrude strand wires, and then cooling, granulating and drying to obtain the composite master batch.
(5) Uniformly mixing the composite master batches and the polypropylene resin material according to the mass ratio of 2:98, feeding the mixture into melt-blowing equipment for melt-blowing spinning, spraying a melt from a screw to a spinning assembly to a spinneret plate, and drawing the melt by high-temperature high-speed airflow to prepare melt-blown superfine fibers;
(6) and (3) winding, electrostatically electret, slitting and rolling the melt-blown superfine fibers to obtain the melt-blown fabric taking flower-shaped graphene as the filler.
Example 4
(1) A high-purity graphite rod is used as an anode, and a platinum electrode is used as a cathode; configuration of KOH/H2O2The electrolyte is an aqueous solution, wherein the concentration of KOH is 5M, and H2O2Is 20 mM.
(2) Putting a high-purity graphite rod and a platinum electrode into an electrolytic cell, adjusting the distance between the electrodes to be 5cm, immersing the graphite rod and the platinum electrode into electrolyte, connecting the high-purity graphite rod and the platinum electrode with a direct-current power supply by using a lead, connecting an anode with the anode of the direct-current power supply, connecting a cathode with the cathode of the direct-current power supply, and carrying out an electrolytic reaction at room temperature after the direct-current power supply applies a direct-current voltage of 15V; after the electrolysis is finished, filtering the electrolyte to obtain a black product, and cleaning the black product by using distilled water;
(3) and drying the cleaned black powder in a drying oven to obtain the flower-shaped graphene.
(4) Weighing flower-shaped graphene, a dispersing agent and a polypropylene resin material according to a mass ratio of 1:1:98, uniformly mixing and stirring, adding into a double-screw extruder, setting the temperature of each section of the extruder to be 150 ℃, starting the extruder to extrude strands, cooling, granulating and drying to obtain the composite master batch.
(5) Uniformly mixing the composite master batches and the polypropylene resin material according to the mass ratio of 5:95, feeding the mixture into melt-blowing equipment for melt-blowing spinning, spraying a melt from a screw to a spinning assembly to a spinneret plate, and drawing the melt by high-temperature high-speed airflow to prepare melt-blown superfine fibers;
(6) and (3) winding, electrostatically electret, slitting and rolling the melt-blown superfine fibers to obtain the melt-blown fabric taking flower-shaped graphene as the filler.
Example 5
(1) A high-purity graphite rod is used as an anode, and a platinum electrode is used as a cathode; configuration of KOH/H2O2The electrolyte is an aqueous solution, wherein the concentration of KOH is 5M, and H2O2Is 20 mM.
(2) Putting a high-purity graphite rod and a platinum electrode into an electrolytic cell, adjusting the distance between the electrodes to be 5cm, immersing the graphite rod and the platinum electrode into electrolyte, connecting the high-purity graphite rod and the platinum electrode with a direct-current power supply by using a lead, connecting an anode with the anode of the direct-current power supply, connecting a cathode with the cathode of the direct-current power supply, and carrying out an electrolytic reaction at room temperature after the direct-current power supply applies a direct-current voltage of 15V; after the electrolysis is finished, filtering the electrolyte to obtain a black product, and cleaning the black product by using distilled water;
(3) and drying the cleaned black powder in a drying oven to obtain the flower-shaped graphene.
(4) Weighing flower-shaped graphene, a dispersing agent and a polypropylene resin material according to a mass ratio of 1:1:98, uniformly mixing and stirring, adding into a double-screw extruder, setting the temperature of each section of the extruder to be 150 ℃, starting the extruder to extrude strands, cooling, granulating and drying to obtain the composite master batch.
(5) Uniformly mixing the composite master batches and the polypropylene resin material according to the mass ratio of 10:90, feeding the mixture into melt-blowing equipment for melt-blowing spinning, spraying a melt from a screw to a spinning assembly to a spinneret plate, and drawing the melt by high-temperature high-speed airflow to prepare melt-blown superfine fibers;
(6) and (3) winding, electrostatically electret, slitting and rolling the melt-blown superfine fibers to obtain the melt-blown fabric taking flower-shaped graphene as the filler.
Comparative example 1
(1) Feeding the polypropylene resin material into melt-blowing equipment to carry out melt-blowing spinning, wherein a melt is fed to a spinning assembly through a screw and then is sprayed out from a spinneret plate, and the melt is drawn by high-temperature high-speed airflow to prepare melt-blown superfine fibers;
(2) and (3) winding, electrostatically electret, slitting and rolling the melt-blown superfine fibers to obtain the melt-blown fabric.
TABLE 1 meltblown properties with addition of flower-like graphene
Note: particulate matter filtration efficiency, pressure differential were tested according to standard YY 0469 + 2011. The antibacterial rate is tested according to the standard GB/T20944.3-2008.
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.
Claims (12)
1. The flower-like graphene is characterized by being composed of a plurality of graphene aggregates which are independent of each other, wherein the graphene aggregates are formed by coiling single-layer or multi-layer ultrathin two-dimensional nano materials, and the size of each single graphene aggregate is 50-200 nm.
2. The flower-like graphene according to claim 1, wherein the graphene aggregate single structure exists at the center of a reel, and is curled into a flower-like structure by a belt-shaped ultrathin two-dimensional nanomaterial around the center of the reel.
3. The flower-like graphene according to claim 1, wherein the number of graphene agglomerate crimp layers is 2-20.
4. A method for preparing flower-like graphene according to any one of claims 1 to 3, comprising the steps of:
(1) a graphite rod is used as an anode, and a metal electrode is used as a cathode;
(2) configuration of KOH/H2O2The aqueous solution is used as electrolyte;
(3) the graphite rod and the metal electrode are used as electrodes of an electrolytic cell and are placed in the electrolytic cell, the electrode position is adjusted, the graphite rod and the metal electrode are immersed in electrolyte, the graphite rod and the metal electrode are connected with a direct current power supply by using a lead, the anode is connected with the anode of the direct current power supply, the cathode is connected with the cathode of the direct current power supply, and after the direct current power supply applies direct current voltage, an electrolytic reaction is carried out;
(4) in the electrolysis process, bubbles are continuously generated on the anode graphite rod, and the color of the electrolyte is changed from colorless to black;
(5) after the electrolysis is finished, filtering the electrolyte to obtain a black product, and cleaning the black product by using distilled water;
(6) and drying the cleaned black powder to obtain the flower-like graphene.
5. The method for preparing flower-like graphene according to claim 4, wherein the concentration of KOH in the step (2) is 0.1M-10M, and H is2O2The concentration of (B) is 10 mM-1M.
6. The method for preparing flower-like graphene according to claim 4, wherein the purity of the graphite rod in the step (3) is not less than 99.9%, the metal anode is a platinum electrode, and the distance between the cathode and the anode is 3-10 cm.
7. The method for preparing flower-like graphene according to claim 1, wherein the direct current voltage in the step (3) is 0.1-20V, and the temperature of the electrolysis reaction system is not higher than 50 ℃.
8. A meltblown fabric, characterized in that the meltblown fibers contain the graphene flower-like particles according to any one of claims 1 to 3, and the graphene flower-like particles are contained in the meltblown fibers in an amount of 0.001 to 1% by mass.
9. A method of making the meltblown fabric of claim 8, comprising the steps of:
(1) preparing the composite master batch: respectively weighing a certain amount of flower-like graphene, a dispersing agent and a polypropylene resin material, uniformly mixing and stirring the three raw materials, adding the mixture into a double-screw extruder, setting the temperature of each interval of the extruder, starting the extruder to extrude strands, and then cooling, granulating and drying to obtain the composite master batch;
(2) and (3) melt-blown process treatment: taking a certain amount of the composite master batch prepared in the step (1) and a certain amount of polypropylene resin material, uniformly mixing the two materials, sending the mixture into melt-blowing equipment for melt-blowing spinning, spraying a melt from a screw to a spinning assembly to a spinneret plate, and drawing the melt by high-temperature high-speed airflow to prepare melt-blown superfine fiber;
(3) performing electret treatment: and (3) winding the melt-blown superfine fibers prepared in the step (2), performing electrostatic electret, slitting and winding to obtain the melt-blown product with flower-like graphene as the filler.
10. The method of making meltblown fabric according to claim 9, wherein: in the step (1), the mass ratio of the flower-shaped graphene to the dispersing agent to the polypropylene resin material is 0.01-10: 0.1-1: 99.89-89; in the step 1, the extrusion temperature is 150-250 ℃.
11. The method of making meltblown fabric according to claim 9, wherein: the mass ratio of the composite master batch to the polypropylene resin material in the step (2) is 0.1-10: 99.9-90; in the step (2), the extrusion temperature is 160-280 ℃, and the receiving distance is 7-25 cm.
12. A mask characterized by using the meltblown fabric of claim 8.
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