CN113186653A - Graphene melt-blown fabric, manufacturing method of graphene melt-blown fabric and mask based on graphene melt-blown fabric - Google Patents
Graphene melt-blown fabric, manufacturing method of graphene melt-blown fabric and mask based on graphene melt-blown fabric Download PDFInfo
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- CN113186653A CN113186653A CN202110457695.6A CN202110457695A CN113186653A CN 113186653 A CN113186653 A CN 113186653A CN 202110457695 A CN202110457695 A CN 202110457695A CN 113186653 A CN113186653 A CN 113186653A
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Images
Classifications
-
- 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
- D04H1/542—Adhesive fibres
- D04H1/544—Olefin series
-
- 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
- A41D13/1192—Protective face masks, e.g. for surgical use, or for use in foul atmospheres with antimicrobial agent
-
- A—HUMAN NECESSITIES
- A41—WEARING APPAREL
- A41D—OUTERWEAR; PROTECTIVE GARMENTS; ACCESSORIES
- A41D31/00—Materials specially adapted for outerwear
- A41D31/02—Layered materials
-
- A—HUMAN NECESSITIES
- A41—WEARING APPAREL
- A41D—OUTERWEAR; PROTECTIVE GARMENTS; ACCESSORIES
- A41D31/00—Materials specially adapted for outerwear
- A41D31/04—Materials specially adapted for outerwear characterised by special function or use
- A41D31/10—Impermeable to liquids, e.g. waterproof; Liquid-repellent
-
- A—HUMAN NECESSITIES
- A41—WEARING APPAREL
- A41D—OUTERWEAR; PROTECTIVE GARMENTS; ACCESSORIES
- A41D31/00—Materials specially adapted for outerwear
- A41D31/04—Materials specially adapted for outerwear characterised by special function or use
- A41D31/12—Hygroscopic; Water retaining
-
- A—HUMAN NECESSITIES
- A41—WEARING APPAREL
- A41D—OUTERWEAR; PROTECTIVE GARMENTS; ACCESSORIES
- A41D31/00—Materials specially adapted for outerwear
- A41D31/04—Materials specially adapted for outerwear characterised by special function or use
- A41D31/30—Antimicrobial, e.g. antibacterial
- A41D31/305—Antimicrobial, e.g. antibacterial using layered materials
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/184—Preparation
- C01B32/19—Preparation by exfoliation
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/198—Graphene oxide
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/30—Active carbon
- C01B32/354—After-treatment
- C01B32/372—Coating; Grafting; Microencapsulation
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
- D01F1/103—Agents inhibiting growth of microorganisms
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/44—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds
- D01F6/46—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds of polyolefins
-
- 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
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- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Textile Engineering (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Materials Engineering (AREA)
- Nanotechnology (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Physical Education & Sports Medicine (AREA)
- General Health & Medical Sciences (AREA)
- Health & Medical Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Filtering Materials (AREA)
- Artificial Filaments (AREA)
- Nonwoven Fabrics (AREA)
Abstract
The invention belongs to the field of melt-blown fabric preparation, and particularly discloses graphene melt-blown fabric, a manufacturing method of the graphene melt-blown fabric and a mask based on the graphene melt-blown fabric, wherein the graphene melt-blown fabric comprises the following raw materials: hydroxylated graphene, activated carbon containing hydroxyl functional groups, antibacterial particles and a polypropylene material; according to the weight percentage, the hydroxylated graphene accounts for 0.05-0.25% of the raw material of the graphene melt-blown fabric, the activated carbon containing hydroxyl functional groups accounts for 0.5-2.5% of the raw material of the graphene melt-blown fabric, the antibacterial particles account for 0.3-1.0% of the raw material of the graphene melt-blown fabric, and the balance is the polypropylene material; the graphene melt-blown fabric disclosed by the invention is low in graphene consumption, good in biocompatibility, low in manufacturing cost, high in mechanical strength, strong in adsorption and antibacterial capabilities, and suitable for manufacturing high-performance masks.
Description
Technical Field
The invention belongs to the field of melt-blown fabric preparation, and particularly discloses graphene melt-blown fabric, a manufacturing method of the graphene melt-blown fabric and a mask based on the graphene melt-blown fabric.
Background
The melt-blown fabric is the most core material of the mask, the melt-blown fabric mainly takes polypropylene as a main raw material, and the fiber diameter can reach 1-5 microns. The superfine fiber with the unique capillary structure increases the number and the surface area of the fiber per unit area, so that the melt-blown fabric has good filtering property, shielding property, heat insulation property and oil absorption property. Can be used in the fields of air and liquid filtering materials, isolating materials, absorbing materials, mask materials, warm-keeping materials, oil absorbing materials, wiping cloth and the like. However, the conventional meltblown fabric has a low mechanical strength, a limited ability to adsorb bacteria and dust, and a limited service life.
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. Arrangement of carbon atoms inside grapheneIn the same sp-form as the graphite monoatomic layer2The hybrid orbit is bonded and has the following characteristics: the carbon atom having 4 valence electrons, 3 of which form sp2Bonds, i.e., each carbon atom contributes an unbound electron located on the pz orbital, the pz orbitals of neighboring atoms perpendicular to the plane can form pi bonds, and the newly formed pi bonds are in a half-filled state. The research proves that the coordination number of carbon atoms in the graphene is 3, the bond length between every two adjacent carbon atoms is 1.42 multiplied by 10-10 meters, and the included angle between bonds is 120 degrees. In addition to the honeycomb layered structure where the sigma bonds are linked to other carbon atoms in hexagonal rings, the pz orbital of each carbon atom perpendicular to the plane of the layer can form a large pi bond (similar to a benzene ring) throughout the multi-atom of the entire layer. Graphene is one of the materials with the highest known strength, has good toughness and can be bent, the theoretical Young modulus of the graphene reaches 1.0TPa, and the inherent tensile strength is 130 GPa. The reduced graphene modified by the hydrogen plasma also has very good strength, and the average modulus can be larger than 0.25 TPa. Therefore, adding graphene addition materials into the melt-blown fabric to enhance the mechanical strength of the melt-blown fabric is a research hotspot at present. For example, CN202011205776.9 (graphene meltblown, a method for manufacturing graphene meltblown, and a mask) in china discloses a graphene meltblown which has excellent antibacterial performance, good adsorption and filtration effects, good dispersion of graphene, and strong adhesion to polypropylene; comprises a graphene material, a block copolymer, modified polypropylene and polypropylene; however, the preparation of the block copolymer and the copolymer itself in the above patent contain styrene, which cannot eliminate the potential hazard to health and is questionable whether to be applied in large scale, and meanwhile, the graphene in the above patent has a large dosage, which is more than 0.3%, and is easy to block a nozzle during melt blowing, so that the block copolymer is needed to assist dispersion, but the preparation is complicated, and the cost is high; china invention]CN202010332424.3 (an in-situ polymerization modified graphene polypropylene meltblown and a preparation method thereof) discloses that the in-situ polymerization modified graphene polypropylene meltblown obtains better mechanical properties, but the preparation method is complex, the graphene dosage is large, and large-scale application is difficult. Therefore how to useThe problem that the existing melt-blown cloth needs to be solved urgently is that a small amount of graphene is used, and the melt-blown cloth with low cost has good mechanical property, good biocompatibility, firmness, durability and strong antibacterial capability.
Disclosure of Invention
In order to overcome the defects, the invention discloses graphene melt-blown fabric, a manufacturing method of the graphene melt-blown fabric and a mask based on the graphene melt-blown fabric. The melt-blown graphene disclosed by the invention is low in consumption, good in biocompatibility, high in mechanical strength, strong in adsorption and antibacterial capacity, and suitable for manufacturing high-performance masks.
The technical scheme of the invention is as follows:
the graphene melt-blown fabric comprises the following raw materials: hydroxylated graphene, activated carbon containing hydroxyl functional groups, antibacterial particles and a polypropylene material; according to the weight percentage, the hydroxylated graphene accounts for 0.05-0.25% of the raw materials of the graphene melt-blown fabric, the activated carbon containing hydroxyl functional groups accounts for 0.5-2.5% of the raw materials of the graphene melt-blown fabric, the antibacterial particles account for 0.3-1.0% of the raw materials of the graphene melt-blown fabric, and the balance is the polypropylene material. Hydroxyl groups on the graphene can be better combined with a polypropylene material, so that the mechanical property of the melt-blown fabric is improved; meanwhile, a large number of hydroxyl functional groups are arranged on the surface of the activated carbon, so that dust and bacteria with various properties can be adsorbed, and the adsorption capacity of the activated carbon is improved; furthermore, antibacterial particles are added, so that the antibacterial and bactericidal effects can be further realized.
Further, according to the graphene meltblown, the percentage of the hydroxylated graphene in the raw materials of the graphene meltblown is 0.1% -0.2%, the percentage of the activated carbon containing hydroxyl functional groups in the raw materials of the graphene meltblown is 1% -2%, the percentage of the antibacterial particles in the raw materials of the graphene meltblown is 0.5% -0.8%, and the balance is the polypropylene material.
Preferably, according to the graphene meltblown, the percentage of the hydroxylated graphene in the raw material of the graphene meltblown is 0.15%, the percentage of the activated carbon containing hydroxyl functional groups in the raw material of the graphene meltblown is 1.5%, the percentage of the antibacterial particles in the raw material of the graphene meltblown is 0.65%, and the balance is the polypropylene material. Experiments of the applicant show that the graphene is less in use amount in the proportion, but the graphene is still excellent in mechanical property and has a good adsorption effect.
Further, the hydroxylated graphene material is prepared by the following steps:
1) preparing graphene oxide: adding concentrated nitric acid into flake graphite powder serving as a raw material; respectively adding potassium permanganate, sodium phosphate and triphenylphosphine oxide at 15-25 deg.C, and stirring for 4-6 h; slowly adding deionized water, stirring for 4-8h, and controlling the temperature within 55-65 ℃; centrifuging at 10000-15000g for 15-30min, washing with water, and drying to obtain graphene oxide powder;
2) preparing hydroxylated graphene: and (2) transferring the graphene oxide powder prepared in the step (1) into a high-pressure reaction kettle filled with mixed gas consisting of inert gas and nitrogen according to the volume ratio of 2:1, controlling the pressure to be 1.5-3.0Mpa and the reaction temperature to be 200-240 ℃ and reacting for 2-4h to obtain the hydroxylated graphene.
Preferably, the hydroxylated graphene material is prepared by the following steps:
1) preparing graphene oxide: adding concentrated nitric acid into flake graphite powder serving as a raw material; respectively adding potassium permanganate, sodium phosphate and triphenylphosphine oxide at 20 ℃, and stirring for 5 h; slowly adding deionized water, stirring for 6h, and controlling the temperature within 60 ℃; centrifuging at 12500g for 25min, washing with water, and drying to obtain graphene oxide powder;
2) preparing hydroxylated graphene: and (2) transferring the graphene oxide powder prepared in the step (1) into a high-pressure reaction kettle filled with mixed gas consisting of inert gas and nitrogen according to the volume ratio of 2:1, controlling the pressure to be 2.5Mpa and the reaction temperature to be 220 ℃, and reacting for 3 hours to obtain the hydroxylated graphene.
Further, the graphene meltblown fabric is prepared by the following steps:
1) dispersing activated carbon into H with mass concentration of 51-55% 2O 2In solution, activated carbon and H 2O 2The mass-to-volume ratio of (A) is 0.1-0.2mg/mL, and stirring is carried out for 10-12 min;
2) ultrasonic treatment is carried out for 1-2h at the temperature of 45-55 ℃, and the power of the ultrasonic treatment is 0.3kW-0.6 kW;
3) filtering, washing with deionized water and carbon tetrachloride until the filtrate is neutral;
4) drying in a vacuum drying oven at 140 deg.C to obtain the active carbon containing hydroxyl functional group.
Preferably, in the graphene meltblown, the activated carbon containing hydroxyl functional groups is prepared by the following steps:
1) dispersing activated carbon to 53 mass percent of H2O 2In solution, activated carbon and H 2O 2The mass-to-volume ratio of (1) is 0.15mg/mL, and stirring is carried out for 11 min;
2) ultrasonic treatment is carried out for 1.5h at the temperature of 50 ℃, and the power of the ultrasonic treatment is 0.45 kW;
3) filtering, washing with deionized water and carbon tetrachloride until the filtrate is neutral;
4) drying in a vacuum drying oven at 140 deg.C to obtain the active carbon containing hydroxyl functional group.
Further, the antibacterial particles of the graphene meltblown are prepared by the following steps:
1): using antibacterial traditional Chinese medicinal materials as natural fiber materials, crushing the natural fiber materials by a crusher, sieving the crushed natural fiber materials with a 100-plus-200-mesh sieve, washing the crushed natural fiber materials with distilled water for three times at normal temperature, then washing the crushed natural fiber materials with absolute ethyl alcohol for two times to remove impurities in the fiber, and drying the washed natural fiber materials for later use;
2): mixing glass fibers and the natural fiber materials dried in the step 1 according to a mass ratio of 1:1, opening the mixture, and carding the mixed fiber materials to form a fluffy net-shaped structure; and drying in dark to obtain the antibacterial particles.
Preferably, the antibacterial traditional Chinese medicinal materials are one or more of truffle, coptis chinensis and dandelion. The chrysosporium fortunei (with the scientific name of Potentilla fructicosa L.) is a shrub plant in the Potentilla of Rosaceae and the height of 2m, the bark of the shrub plant is longitudinally peeled off, the recent research shows that the extract of the chrysosporium fortunei has strong antibacterial effect, and the application report of the chrysosporium fortunei in melt-blown cloth is not found at present. Coptis chinensis, (academic name: Coptis chinensis Franch.) alias: rhizoma Coptidis, and rhizoma Coptidis belonging to Ranunculaceae, and containing alkaloids such as berberine, coptisine, methyl coptisine, and tetrandrine, with obvious bactericidal effect. Taraxacum mongolicum hand-Mazz (Latin name) is used as a botanical, and Taraxacum mongolicum hand-held, is used as a perennial herb of Taraxacum, and has bactericidal effect and fragrant taste. The antibacterial granules prepared by crosslinking the natural plant fibers of the traditional Chinese medicinal materials and the artificial glass fibers have the advantages of large specific surface area, strong adsorption and sterilization capabilities and natural thinking, and after the antibacterial granules are prepared into the melt-blown cloth, the melt-blown cloth has better adsorption and sterilization capabilities, natural fragrance and good biocompatibility, and is suitable for being applied to close-fitting fabrics, particularly masks.
Further, the graphene meltblown fabric is a polypropylene modified composite material and is prepared from the following raw materials in parts by weight: polypropylene: 100 parts of perfluoroacrylate: 5-10 parts of glass fiber: 4-8 parts of polypropylene grafted maleic anhydride: 2-4 parts of a silane coupling agent: 1-2%, antioxidant: 0.2-0.5 parts of lubricant: 0.2 to 0.4 portion. The common polypropylene material is modified, and the glass fiber is added on the basis of keeping the excellent performance of the polypropylene to prepare the long fiber reinforced polypropylene modified composite material, so that the mechanical strength of the melt-blown fabric is further enhanced, the service life of the melt-blown fabric is prolonged, and the waterproof performance of the melt-blown fabric is improved.
Preferably, the polypropylene material of the graphene meltblown is a polypropylene modified composite material and is composed of the following raw materials in parts by weight: polypropylene: 100 parts of perfluoroacrylate: 7.5 parts, glass fiber: 6 parts of polypropylene grafted maleic anhydride: 3 parts, silane coupling agent: 1.5%, antioxidant: 0.35 part, lubricant: 0.3 part.
Further, the graphene meltblown fabric is prepared from a polypropylene modified composite material by the following steps:
1) uniformly mixing the raw materials: uniformly mixing polypropylene, perfluoroacrylate, polypropylene grafted maleic anhydride, a silane coupling agent, an antioxidant and a lubricant in a mixer according to a ratio;
2) feeding glass fibers: adding glass fiber from a glass fiber inlet of a double-screw extruder;
3) mixing in a double-screw extruder: adding the mixture obtained in the step 1 into a double-screw extruder to be mixed with glass fibers, wherein the temperature of the double-screw extruder is set to be between 190 and 210 ℃, and the screw rotating speed of the double-screw extruder is 400-500 rpm;
4) and extruding the obtained material, cooling and granulating to obtain the polypropylene modified composite material.
The second aspect of the invention is illustrated below:
the manufacturing method of the graphene melt-blown fabric comprises the following steps:
1) uniformly mixing hydroxylated graphene, activated carbon containing hydroxyl functional groups and a polypropylene material according to the formula amount to obtain a mixture A;
2) adding the antibacterial particles with the formula amount into the mixture A in the step 1, and uniformly mixing to obtain a melt-blown fabric raw material B;
3) adding the melt-blown cloth raw material B prepared in the step 2 into a screw extruder for melting treatment, wherein the screw extruder is provided with 4 zones with gradually increased temperature, setting the temperature of each zone to a process required value, preserving the temperature for 30min, and conveying a melt obtained by melting to a spinning assembly by adopting a metering pump;
4) and (3) sequentially opening the main machine, the fan and the receiving net curtain, blowing hot air of the fan, opening a wind-up roll and an electret voltage after the meltblown fabric is normally sprayed out, and rolling and molding the wind-up roll to obtain a finished meltblown fabric product. The method for preparing the graphene melt-blown fabric has the advantages of short preparation process, sectional temperature control to keep the pressure of the material constant, good graphene dispersion performance, difficulty in blocking a spray head and cost saving.
Further, in the above manufacturing method of the graphene meltblown fabric, in step 3, the temperature values of the 4 zones are respectively: the temperature in the first zone was 175 deg.C, the temperature in the second zone was 200 deg.C, the temperature in the third zone was 230 deg.C, and the temperature in the fourth zone was 250 deg.C.
The third aspect of the present invention is explained below:
the utility model provides a mask, the mask includes close skin layer, interior water absorption layer, antibacterial adsorbed layer, outer shaping layer, outer waterproof layer, antibacterial adsorbed layer is formed by the preparation of above-mentioned graphite alkene melt-blown cloth.
According to the technical scheme, the invention has the following beneficial effects:
1. hydroxyl groups on the graphene used in the invention can be better combined with a polypropylene material, so that the mechanical property of the melt-blown fabric is improved; meanwhile, a large number of hydroxyl functional groups are arranged on the surface of the activated carbon, so that dust and bacteria with various properties can be adsorbed, and the adsorption capacity of the activated carbon is improved; furthermore, antibacterial particles are added, so that the antibacterial and bactericidal effects of the melt-blown fabric are further improved.
2. The antibacterial granules prepared by crosslinking natural plant fibers in the traditional Chinese medicinal materials and artificial glass fibers have large specific surface area, strong adsorption and sterilization capabilities and natural fragrance, and the fused spray cloth has better bacteria adsorption and sterilization capabilities and natural fragrance and good biocompatibility and is suitable for being applied to close-fitting fabrics, particularly masks.
3. The invention modifies the common polypropylene material, and adds the glass fiber to prepare the long fiber reinforced polypropylene modified composite material on the basis of keeping the excellent performance of the polypropylene, thereby further enhancing the mechanical strength of the melt-blown fabric, prolonging the service life of the melt-blown fabric and improving the waterproof performance of the melt-blown fabric.
4. The graphene melt-blown fabric prepared by the preparation method has the advantages of short preparation process, capability of keeping the pressure of the material constant by segmented temperature control, good graphene dispersion performance, difficulty in blocking a spray head, simplicity in equipment maintenance and cost saving.
Drawings
FIG. 1 is a schematic view of a mask made in accordance with the present invention in layers;
wherein: the skin-friendly layer comprises a skin-friendly layer 10, an internal water absorption layer 20, a bacteriostatic absorption layer 30, an outer forming layer 40 and an outer waterproof layer 50.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. 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 experimental materials are commercially available without specific indication.
Example 1
The graphene melt-blown fabric comprises the following raw materials: hydroxylated graphene, activated carbon containing hydroxyl functional groups, antibacterial particles and a polypropylene material; according to the weight percentage, the percentage of the hydroxylated graphene in the raw material of the graphene melt-blown fabric is 0.05%, the percentage of the activated carbon containing hydroxyl functional groups in the raw material of the graphene melt-blown fabric is 0.5%, the percentage of the antibacterial particles in the raw material of the graphene melt-blown fabric is 0.3%, and the balance is the polypropylene material.
The antibacterial particles are prepared by the following steps:
1): taking an antibacterial Chinese medicinal material, namely the whole plant of the gynura divaricata, as a natural fiber material, crushing the natural fiber material by a crusher, sieving the crushed natural fiber material by a sieve with 100-mesh and 200-mesh, washing the crushed natural fiber material by distilled water for three times at normal temperature, then using absolute ethyl alcohol for two times to remove impurities in the fiber, and drying the fiber for later use;
2): mixing glass fibers and the natural fiber materials dried in the step 1 according to a mass ratio of 1:1, opening the mixture, and carding the mixed fiber materials to form a fluffy net-shaped structure; and drying in dark to obtain the antibacterial particles.
Example 2
The graphene melt-blown fabric comprises the following raw materials: hydroxylated graphene, activated carbon containing hydroxyl functional groups, antibacterial particles and a polypropylene material; according to the weight percentage, the percentage of the hydroxylated graphene in the raw material of the graphene melt-blown fabric is 0.1%, the percentage of the activated carbon containing hydroxyl functional groups in the raw material of the graphene melt-blown fabric is 1%, the percentage of the antibacterial particles in the raw material of the graphene melt-blown fabric is 0.5%, and the balance is the polypropylene material.
The antibacterial particles are prepared by the following steps:
1): taking the whole plant of antibacterial traditional Chinese medicines of the gynura divaricata and the coptis chinensis (the mass ratio is 1: 1) as a natural fiber material, crushing the natural fiber material by a crusher, sieving the crushed natural fiber material by a sieve with 100-plus-200 meshes, washing the crushed natural fiber material by distilled water for three times at normal temperature, then using absolute ethyl alcohol for two times to remove impurities in the fiber, and drying the obtained product for later use;
2): mixing glass fibers and the natural fiber materials dried in the step 1 according to a mass ratio of 1:1, opening the mixture, and carding the mixed fiber materials to form a fluffy net-shaped structure; and drying in dark to obtain the antibacterial particles.
Example 3
The graphene melt-blown fabric comprises the following raw materials: hydroxylated graphene, activated carbon containing hydroxyl functional groups, antibacterial particles and a polypropylene material; according to the weight percentage, the percentage of the hydroxylated graphene in the raw material of the graphene melt-blown fabric is 0.15%, the percentage of the activated carbon containing hydroxyl functional groups in the raw material of the graphene melt-blown fabric is 1.5%, the percentage of the antibacterial particles in the raw material of the graphene melt-blown fabric is 0.65%, and the balance is the polypropylene material.
The antibacterial particles are prepared by the following steps:
1): taking antibacterial Chinese medicinal materials of the Jinlumei, the coptis root and the dandelion (the mass ratio is 1: 1: 1) as whole plants as natural fiber materials, crushing the natural fiber materials by a crusher, sieving the crushed natural fiber materials by a 100-mesh and 200-mesh sieve, washing the crushed natural fiber materials by distilled water for three times at normal temperature, then washing the crushed natural fiber materials by absolute ethyl alcohol for two times to remove impurities in the fiber, and drying the washed natural fiber materials for later use;
2): mixing glass fibers and the natural fiber materials dried in the step 1 according to a mass ratio of 1:1, opening the mixture, and carding the mixed fiber materials to form a fluffy net-shaped structure; and drying in dark to obtain the antibacterial particles.
Example 4
The graphene melt-blown fabric comprises the following raw materials: hydroxylated graphene, activated carbon containing hydroxyl functional groups, antibacterial particles and a polypropylene material; according to the weight percentage, the percentage of the hydroxylated graphene in the raw material of the graphene melt-blown fabric is 0.2%, the percentage of the activated carbon containing hydroxyl functional groups in the raw material of the graphene melt-blown fabric is 2%, the percentage of the antibacterial particles in the raw material of the graphene melt-blown fabric is 0.8%, and the balance is the polypropylene material.
The antibacterial particles are prepared by the following steps:
1): taking the whole plant of the antibacterial traditional Chinese medicine coptis as a natural fiber material, crushing the natural fiber material by a crusher, sieving the crushed natural fiber material by a sieve with 100 meshes and 200 meshes, washing the crushed natural fiber material by distilled water for three times at normal temperature, then washing the crushed natural fiber material by absolute ethyl alcohol for two times to remove impurities in the fiber, and drying the washed natural fiber material for later use;
2): mixing glass fibers and the natural fiber materials dried in the step 1 according to a mass ratio of 1:1, opening the mixture, and carding the mixed fiber materials to form a fluffy net-shaped structure; and drying in dark to obtain the antibacterial particles.
Example 5
The graphene melt-blown fabric comprises the following raw materials: hydroxylated graphene, activated carbon containing hydroxyl functional groups, antibacterial particles and a polypropylene material; according to the weight percentage, the percentage of the hydroxylated graphene in the raw material of the graphene melt-blown fabric is 0.25%, the percentage of the activated carbon containing hydroxyl functional groups in the raw material of the graphene melt-blown fabric is 2.5%, the percentage of the antibacterial particles in the raw material of the graphene melt-blown fabric is 1.0%, and the balance is the polypropylene material.
The antibacterial particles are prepared by the following steps:
1): taking the whole plants of antibacterial Chinese medicinal materials of coptis chinensis and dandelion (the mass ratio is 1: 1) as natural fiber materials, crushing the natural fiber materials by a crusher, sieving the crushed natural fiber materials by a sieve with 100-mesh and 200-mesh, washing the crushed natural fiber materials by distilled water for three times at normal temperature, then using absolute ethyl alcohol for two times to remove impurities in the fiber, and drying the washed natural fiber materials for later use;
2): mixing glass fibers and the natural fiber materials dried in the step 1 according to a mass ratio of 1:1, opening the mixture, and carding the mixed fiber materials to form a fluffy net-shaped structure; and drying in dark to obtain the antibacterial particles.
Example 6
Polypropylene modification 1
The graphene melt-blown fabric comprises the following raw materials: hydroxylated graphene, activated carbon containing hydroxyl functional groups, antibacterial particles and a polypropylene material; according to the weight percentage, the percentage of the hydroxylated graphene in the raw material of the graphene melt-blown fabric is 0.15%, the percentage of the activated carbon containing hydroxyl functional groups in the raw material of the graphene melt-blown fabric is 1.5%, the percentage of the antibacterial particles in the raw material of the graphene melt-blown fabric is 0.65%, and the balance is the polypropylene material.
The antibacterial particles are prepared by the following steps:
1): taking antibacterial Chinese medicinal materials of the Jinlumei, the coptis root and the dandelion (the mass ratio is 1: 1: 1) as whole plants as natural fiber materials, crushing the natural fiber materials by a crusher, sieving the crushed natural fiber materials by a 100-mesh and 200-mesh sieve, washing the crushed natural fiber materials by distilled water for three times at normal temperature, then washing the crushed natural fiber materials by absolute ethyl alcohol for two times to remove impurities in the fiber, and drying the washed natural fiber materials for later use;
2): mixing glass fibers and the natural fiber materials dried in the step 1 according to a mass ratio of 1:1, opening the mixture, and carding the mixed fiber materials to form a fluffy net-shaped structure; and drying in dark to obtain the antibacterial particles.
The polypropylene material is a polypropylene modified composite material and is composed of the following raw materials in parts by weight: polypropylene: 100 parts of perfluoroacrylate: 5 parts, glass fiber: 4 parts of polypropylene grafted maleic anhydride: 2 parts, silane coupling agent: 1% of antioxidant: 0.2 part, lubricant: 0.2 part.
The propylene modified composite material is prepared by the following steps:
1) uniformly mixing the raw materials: uniformly mixing polypropylene, perfluoroacrylate, polypropylene grafted maleic anhydride, a silane coupling agent, an antioxidant and a lubricant in a mixer according to a ratio;
2) feeding glass fibers: adding glass fiber from a glass fiber inlet of a double-screw extruder;
3) mixing in a double-screw extruder: adding the mixture obtained in the step 1 into a double-screw extruder, and mixing the mixture and glass fibers together, wherein the temperature of the double-screw extruder is set at 190 ℃, and the screw rotating speed of the double-screw extruder is 400 rpm;
4) and extruding the obtained material, cooling and granulating to obtain the polypropylene modified composite material.
Example 7
Polypropylene modification 2
The graphene melt-blown fabric comprises the following raw materials: hydroxylated graphene, activated carbon containing hydroxyl functional groups, antibacterial particles and a polypropylene material; according to the weight percentage, the percentage of the hydroxylated graphene in the raw material of the graphene melt-blown fabric is 0.15%, the percentage of the activated carbon containing hydroxyl functional groups in the raw material of the graphene melt-blown fabric is 1.5%, the percentage of the antibacterial particles in the raw material of the graphene melt-blown fabric is 0.65%, and the balance is the polypropylene material.
The antibacterial particles are prepared by the following steps:
1): taking antibacterial Chinese medicinal materials of the Jinlumei, the coptis root and the dandelion (the mass ratio is 1: 1: 1) as whole plants as natural fiber materials, crushing the natural fiber materials by a crusher, sieving the crushed natural fiber materials by a 100-mesh and 200-mesh sieve, washing the crushed natural fiber materials by distilled water for three times at normal temperature, then washing the crushed natural fiber materials by absolute ethyl alcohol for two times to remove impurities in the fiber, and drying the washed natural fiber materials for later use;
2): mixing glass fibers and the natural fiber materials dried in the step 1 according to a mass ratio of 1:1, opening the mixture, and carding the mixed fiber materials to form a fluffy net-shaped structure; and drying in dark to obtain the antibacterial particles.
The polypropylene material is a polypropylene modified composite material and is composed of the following raw materials in parts by weight: polypropylene: 100 parts of perfluoroacrylate: 7.5 parts, glass fiber: 6 parts of polypropylene grafted maleic anhydride: 3 parts, silane coupling agent: 1.5%, antioxidant: 0.35 part, lubricant: 0.3 part.
The propylene modified composite material is prepared by the following steps:
1) uniformly mixing the raw materials: uniformly mixing polypropylene, perfluoroacrylate, polypropylene grafted maleic anhydride, a silane coupling agent, an antioxidant and a lubricant in a mixer according to a ratio;
2) feeding glass fibers: adding glass fiber from a glass fiber inlet of a double-screw extruder;
3) mixing in a double-screw extruder: adding the mixture obtained in the step 1 into a double-screw extruder, and mixing the mixture and glass fibers together, wherein the temperature of the double-screw extruder is set at 200 ℃, and the screw rotating speed of the double-screw extruder is 450 rpm;
4) and extruding the obtained material, cooling and granulating to obtain the polypropylene modified composite material.
Example 8
Modification of Polypropylene 3
The graphene melt-blown fabric comprises the following raw materials: hydroxylated graphene, activated carbon containing hydroxyl functional groups, antibacterial particles and a polypropylene material; according to the weight percentage, the percentage of the hydroxylated graphene in the raw material of the graphene melt-blown fabric is 0.15%, the percentage of the activated carbon containing hydroxyl functional groups in the raw material of the graphene melt-blown fabric is 1.5%, the percentage of the antibacterial particles in the raw material of the graphene melt-blown fabric is 0.65%, and the balance is the polypropylene material.
The antibacterial particles are prepared by the following steps:
1): taking antibacterial Chinese medicinal materials of the Jinlumei, the coptis root and the dandelion (the mass ratio is 1: 1: 1) as whole plants as natural fiber materials, crushing the natural fiber materials by a crusher, sieving the crushed natural fiber materials by a 100-mesh and 200-mesh sieve, washing the crushed natural fiber materials by distilled water for three times at normal temperature, then washing the crushed natural fiber materials by absolute ethyl alcohol for two times to remove impurities in the fiber, and drying the washed natural fiber materials for later use;
2): mixing glass fibers and the natural fiber materials dried in the step 1 according to a mass ratio of 1:1, opening the mixture, and carding the mixed fiber materials to form a fluffy net-shaped structure; and drying in dark to obtain the antibacterial particles.
The polypropylene material is a polypropylene modified composite material and is composed of the following raw materials in parts by weight: polypropylene: 100 parts of perfluoroacrylate: 10 parts, glass fiber: 8 parts of polypropylene grafted maleic anhydride: 4 parts, silane coupling agent: 2%, antioxidant: 0.5 part, lubricant: 0.4 part.
The propylene modified composite material is prepared by the following steps:
1) uniformly mixing the raw materials: uniformly mixing polypropylene, perfluoroacrylate, polypropylene grafted maleic anhydride, a silane coupling agent, an antioxidant and a lubricant in a mixer according to a ratio;
2) feeding glass fibers: adding glass fiber from a glass fiber inlet of a double-screw extruder;
3) mixing in a double-screw extruder: adding the mixture obtained in the step 1 into a double-screw extruder, and mixing the mixture and glass fibers together, wherein the temperature of the double-screw extruder is set at 210 ℃, and the screw rotating speed of the double-screw extruder is 500 rpm;
4) and extruding the obtained material, cooling and granulating to obtain the polypropylene modified composite material.
Example 9
Examples of preparation of meltblown
Graphene meltblown fabrics were prepared according to the formulations of examples 1-8,
1) uniformly mixing hydroxylated graphene, activated carbon containing hydroxyl functional groups and a polypropylene material according to the formula amount to obtain a mixture A;
2) adding the antibacterial particles with the formula amount into the mixture A in the step 1, and uniformly mixing to obtain a melt-blown fabric raw material B;
3) and (3) adding the melt-blown fabric raw material B prepared in the step (2) into a screw extruder for melting treatment, wherein the screw extruder is provided with 4 zones with gradually increased temperature, and the temperature of each zone is set to a process required value (the temperature values of the 4 zones are respectively: the temperature of the first zone is 175 ℃, the temperature of the second zone is 200 ℃, the temperature of the third zone is 230 ℃, the temperature of the fourth zone is 250 ℃) and the temperature is kept for 30min, and a melt obtained by melting is sent to a spinning pack by adopting a metering pump;
4) and (3) sequentially opening the main machine, the fan and the receiving net curtain, blowing hot air of the fan, opening a wind-up roll and an electret voltage after the meltblown fabric is normally sprayed out, and rolling and molding the wind-up roll to obtain a finished meltblown fabric product.
Wherein the hydroxylated graphene material is prepared by the following steps:
1) preparing graphene oxide: adding concentrated nitric acid with the mass of 2 times of that of graphite powder into flake graphite powder serving as a raw material; then respectively adding 0.1 time of potassium permanganate, 0.2 time of sodium phosphate and 0.2 time of triphenylphosphine oxide by mass at the temperature of 20 ℃, and stirring for 5 hours; slowly adding deionized water, stirring for 6h, and controlling the temperature within 60 ℃; centrifuging at 12500g for 25min, washing with water, and drying to obtain graphene oxide powder;
2) preparing hydroxylated graphene: and (2) transferring the graphene oxide powder prepared in the step (1) into a high-pressure reaction kettle filled with mixed gas consisting of helium and nitrogen in a volume ratio of 2:1, controlling the pressure to be 2.5Mpa and the reaction temperature to be 220 ℃, and reacting for 3 hours to obtain the hydroxylated graphene.
Wherein the activated carbon containing hydroxyl functional groups is prepared by the following steps:
1) dispersing activated carbon to 53 mass percent of H 2O 2In solution, activated carbon and H 2O 2The mass-to-volume ratio of (1) is 0.15mg/mL, and stirring is carried out for 11 min;
2) ultrasonic treatment is carried out for 1.5h at the temperature of 50 ℃, and the power of the ultrasonic treatment is 0.45 kW;
3) filtering, washing with deionized water and carbon tetrachloride until the filtrate is neutral;
4) drying in a vacuum drying oven at 140 deg.C to obtain the active carbon containing hydroxyl functional group.
Comparative example 1
The raw materials of the graphene melt-blown fabric are the same as those in example 3, and the preparation method is the same as that in example 9 except that ordinary graphene is substituted for hydroxylated graphene.
Comparative example 2
The raw materials of the graphene melt-blown fabric are the same as those in example 3, and the preparation method is the same as that in example 9, except that ordinary graphene is used for replacing hydroxylated graphene, and no activated carbon is contained.
Comparative example 3
The raw materials of the graphene melt-blown fabric are the same as those in example 3, and the preparation method is the same as that in example 9, except that ordinary graphene is used for replacing hydroxylated graphene, and activated carbon and antibacterial particles are not contained.
Comparative example 4
The common melt-blown fabric sold in the market does not contain graphene.
Test example 1
Comparative test of meltblown fabric properties
The meltblown fabrics prepared in examples 1 to 8 and comparative examples 1 to 3 and the conventional meltblown fabric commercially available in comparative example 4 were subjected to the following performance tests
(1) Meltblown transverse/machine direction breaking force (MD/CD) test reference standard FZ/T60005.
(2) The melt-blown fabric Particle Filtration Efficiency (PFE) and resistance test refers to the standard YY0469-2011, and the specific test condition is that the flow is 85L/min and the single layer is adopted.
(3) The long-term performance of the meltblown was evaluated by ageing tests, in particular with reference to the standard GB/T32610-.
The test data are shown in tables 1-3 below, and tables 2 and 3 are the continuation of table 1 due to the large number of entries.
Table 1 test data table, examples 1-5.
| Example 1 | Example 2 | Example 3 | Example 4 | Example 5 | |
| Meltblown transverse rupture Strength (MD) | 35.2 | 35.6 | 36.1 | 36.5 | 36.7 |
| Meltblown longitudinal breaking strength (CD) | 16.3 | 16.4 | 16.6 | 17.1 | 17.3 |
| Melt blown cloth Particle Filtration Efficiency (PFE) | 97.3 | 97.4 | 97.5 | 97.2 | 97.6 |
| Resistance test, Pa | 28 | 27 | 27 | 28 | 29 |
| PPE after aging | 97.1 | 97.0 | 97.2 | 96.9 | 97.3 |
Table 2 test data table, examples 6-8, comparative examples 1-2.
| Example 6 | Example 7 | Example 8 | Comparative example 1 | Comparative example 2 | |
| Meltblown transverse rupture Strength (MD) | 37.4 | 38.3 | 38.7 | 34.1 | 32.2 |
| Meltblown longitudinal breaking strength (CD) | 17.9 | 18.2 | 18.4 | 15.2 | 14.1 |
| Melt blown cloth Particle Filtration Efficiency (PFE) | 97.9 | 98.3 | 98.8 | 95.1 | 94.2 |
| Resistance test, Pa | 29 | 30 | 31 | 29 | 28 |
| PPE after aging | 97.4 | 97.6 | 97.9 | 92.1 | 91.2 |
Table 3 test data table, comparative examples 3-4.
| Comparative example 3 | Comparative example 4 | |
| Meltblown transverse rupture Strength (MD) | 31.1 | 30.2 |
| Meltblown longitudinal breaking strength (CD) | 13.9 | 12.5 |
| Melt blown cloth Particle Filtration Efficiency (PFE) | 93.9 | 92.1 |
| Resistance test, Pa | 26 | 28 |
| PPE after aging | 90.9 | 88.1 |
From the above data tables 1-3, it can be concluded that the melt-blown fabric produced within the range of the amounts of the components of the present invention has a good balance of PFE, aging resistance, and strength, and is significantly improved compared to the comparative ratio.
Test example 2
And (5) carrying out comparison test on the filtering, sterilizing and antiviral abilities of the mask.
The masks prepared from the melt-blown cloths of the above examples 1-8 and comparative examples 1-4 have the structure shown in figure 1, and comprise a skin-friendly layer 10, an internal water absorption layer 20, a bacteriostatic adsorption layer 30, an external forming layer 40 and an external waterproof layer 50, wherein the bacteriostatic adsorption layer 30 is prepared from the melt-blown cloth.
The mask prepared by the above example is subjected to filtration performance evaluation and comparison according to the standard of YY0469-2011 medical surgical mask technical requirement, and on the basis of the general bacterial filtration index, the new coronavirus surface S protein is particularly fixed on SiO with the same size2The surfaces of the nanospheres are used for simulating a virus particle aerosol filtration experiment, the active antiviral performance effect of the mask is inspected, and the test parameters and results are shown in table 4.
Table 4 comparative test data of filtration, sterilization and antiviral ability of mask.
| Bacterial filtration efficiency BFE (%) | Fine particle filtration efficiency PEF (%) | Respiratory resistance (Pa) | Novel coronavirus mimic particles | |
| Example 1 | 97.5 | 98.3 | 39 | 99.1 |
| Example 2 | 97.5 | 98.4 | 39 | 99.3 |
| Example 3 | 97.6 | 98.7 | 40 | 99.4 |
| Example 4 | 97.8 | 98.3 | 38 | 99.3 |
| Example 5 | 97.1 | 98.5 | 41 | 99.2 |
| Example 6 | 98.1 | 99.1 | 38 | 99.7 |
| Example 7 | 98.2 | 99.4 | 37 | 99.8 |
| Example 8 | 98.1 | 99.2 | 39 | 99.6 |
| Comparative example 1 | 96.2 | 97.3 | 38 | 97.1 |
| Comparative example 2 | 96.7 | 97.1 | 38 | 96.9 |
| Comparative example 3 | 96.5 | 97.5 | 36 | 96.6 |
| Comparative example 4 | 93.2 | 94.4 | 40 | 94.9 |
The following conclusion can be drawn from the data table, and compared with the comparative example, the mask made of the graphene meltblown disclosed by the invention has the advantages that the bacterial filtration efficiency, the particulate filtration efficiency and the filtration efficiency of the new coronavirus simulation particles are obviously improved.
The above are only preferred embodiments of the present invention, and the scope of the present invention should not be limited thereby, and all the equivalent changes and modifications made by the claims and the summary of the invention should be covered by the protection scope of the present patent application.
Claims (10)
1. The graphene meltblown is characterized in that raw materials of the graphene meltblown consist of the following components: hydroxylated graphene, activated carbon containing hydroxyl functional groups, antibacterial particles and a polypropylene material; according to the weight percentage, the hydroxylated graphene accounts for 0.05-0.25% of the raw materials of the graphene melt-blown fabric, the activated carbon containing hydroxyl functional groups accounts for 0.5-2.5% of the raw materials of the graphene melt-blown fabric, the antibacterial particles account for 0.3-1.0% of the raw materials of the graphene melt-blown fabric, and the balance is the polypropylene material.
2. The graphene meltblown according to claim 1, wherein the hydroxylated graphene accounts for 0.1-0.2% of the raw materials of the graphene meltblown, the activated carbon containing hydroxyl functional groups accounts for 1-2% of the raw materials of the graphene meltblown, the antibacterial particles account for 0.5-0.8% of the raw materials of the graphene meltblown, and the balance is the polypropylene material.
3. The graphene meltblown according to claim 1, wherein the hydroxylated graphene material is prepared by:
1) preparing graphene oxide: adding concentrated nitric acid into flake graphite powder serving as a raw material; respectively adding potassium permanganate, sodium phosphate and triphenylphosphine oxide at 15-25 deg.C, and stirring for 4-6 h; slowly adding deionized water, stirring for 4-8h, and controlling the temperature within 55-65 ℃; centrifuging at 10000-15000g for 15-30min, washing with water, and drying to obtain graphene oxide powder;
2) preparing hydroxylated graphene: and (2) transferring the graphene oxide powder prepared in the step (1) into a high-pressure reaction kettle filled with mixed gas consisting of inert gas and nitrogen according to the volume ratio of 2:1, controlling the pressure to be 1.5-3.0Mpa and the reaction temperature to be 200-240 ℃ and reacting for 2-4h to obtain the hydroxylated graphene.
4. The graphene meltblown of claim 1, wherein the hydroxyl functional group-containing activated carbon is prepared by:
1) dispersing activated carbon into H with mass concentration of 51-55%2O 2In solution, activated carbon and H 2O 2The mass-to-volume ratio of (A) is 0.1-0.2mg/mL, and stirring is carried out for 10-12 min;
2) ultrasonic treatment is carried out for 1-2h at the temperature of 45-55 ℃, and the power of the ultrasonic treatment is 0.3kW-0.6 kW;
3) filtering, washing with deionized water and carbon tetrachloride until the filtrate is neutral;
4) drying in a vacuum drying oven at 140 deg.C to obtain the active carbon containing hydroxyl functional group.
5. The graphene meltblown of claim 1, wherein the antimicrobial particles are prepared by:
1): using antibacterial traditional Chinese medicinal materials as natural fiber materials, crushing the natural fiber materials by a crusher, sieving the crushed natural fiber materials with a 100-plus-200-mesh sieve, washing the crushed natural fiber materials with distilled water for three times at normal temperature, then washing the crushed natural fiber materials with absolute ethyl alcohol for two times to remove impurities in the fiber, and drying the washed natural fiber materials for later use;
2): mixing glass fibers and the natural fiber materials dried in the step 1 according to a mass ratio of 1:1, opening the mixture, and carding the mixed fiber materials to form a fluffy net-shaped structure; and drying in dark to obtain the antibacterial particles.
6. The graphene meltblown according to claim 1, wherein the polypropylene material is a polypropylene modified composite material and is composed of the following raw materials in parts by weight: polypropylene: 100 parts of perfluoroacrylate: 5-10 parts of glass fiber: 4-8 parts of polypropylene grafted maleic anhydride: 2-4 parts of a silane coupling agent: 1-2%, antioxidant: 0.2-0.5 parts of lubricant: 0.2 to 0.4 portion.
7. The graphene meltblown according to claim 6, wherein the propylene-modified composite material is prepared by:
1) uniformly mixing the raw materials: uniformly mixing polypropylene, perfluoroacrylate, polypropylene grafted maleic anhydride, a silane coupling agent, an antioxidant and a lubricant in a mixer according to a ratio;
2) feeding glass fibers: adding glass fiber from a glass fiber inlet of a double-screw extruder;
3) mixing in a double-screw extruder: adding the mixture obtained in the step 1 into a double-screw extruder to be mixed with glass fibers, wherein the temperature of the double-screw extruder is set to be between 190 and 210 ℃, and the screw rotating speed of the double-screw extruder is 400-500 rpm;
4) and extruding the obtained material, cooling and granulating to obtain the polypropylene modified composite material.
8. The method of making the graphene meltblown fabric of any one of claims 1-7, comprising the steps of:
1) uniformly mixing hydroxylated graphene, activated carbon containing hydroxyl functional groups and a polypropylene material according to the formula amount to obtain a mixture A;
2) adding the antibacterial particles with the formula amount into the mixture A in the step 1, and uniformly mixing to obtain a melt-blown fabric raw material B;
3) adding the melt-blown cloth raw material B prepared in the step 2 into a screw extruder for melting treatment, wherein the screw extruder is provided with 4 zones with gradually increased temperature, setting the temperature of each zone to a process required value, preserving the temperature for 30min, and conveying a melt obtained by melting to a spinning assembly by adopting a metering pump;
4) and (3) sequentially opening the main machine, the fan and the receiving net curtain, blowing hot air of the fan, opening a wind-up roll and an electret voltage after the meltblown fabric is normally sprayed out, and rolling and molding the wind-up roll to obtain a finished meltblown fabric product.
9. The method according to claim 8, wherein in step 3, the temperature values of 4 zones are respectively: the temperature in the first zone was 175 deg.C, the temperature in the second zone was 200 deg.C, the temperature in the third zone was 230 deg.C, and the temperature in the fourth zone was 250 deg.C.
10. A mask, the mask comprises a skin-friendly layer (10), an inner water absorption layer (20), a bacteriostatic adsorption layer (30), an outer molding layer (40) and an outer waterproof layer (50), and is characterized in that the bacteriostatic adsorption layer (30) is made of the graphene melt-blown fabric as claimed in any one of claims 1 to 7.
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