CN114369323A - Plant-source sunlight-driven efficient antibacterial and antiviral multilayer composite nanofiber protective material and preparation method and application thereof - Google Patents

Plant-source sunlight-driven efficient antibacterial and antiviral multilayer composite nanofiber protective material and preparation method and application thereof Download PDF

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CN114369323A
CN114369323A CN202210069841.2A CN202210069841A CN114369323A CN 114369323 A CN114369323 A CN 114369323A CN 202210069841 A CN202210069841 A CN 202210069841A CN 114369323 A CN114369323 A CN 114369323A
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composite nanofiber
protective material
multilayer composite
high molecular
layer
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CN114369323B (en
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周武艺
陈品鸿
张声森
杨志
黄子蕴
卞永双
谢晓琪
吕芷薇
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South China Agricultural University
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B27/00—Layered products comprising a layer of synthetic resin
    • B32B27/06—Layered products comprising a layer of synthetic resin as the main or only constituent of a layer, which is next to another layer of the same or of a different material
    • A—HUMAN NECESSITIES
    • A41—WEARING APPAREL
    • A41D—OUTERWEAR; PROTECTIVE GARMENTS; ACCESSORIES
    • A41D1/00—Garments
    • 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B33/00—Layered products characterised by particular properties or particular surface features, e.g. particular surface coatings; Layered products designed for particular purposes not covered by another single class
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00—Formation of filaments, threads, or the like
    • D01D5/0007—Electro-spinning
    • D01D5/0015—Electro-spinning characterised by the initial state of the material
    • D01D5/003—Electro-spinning characterised by the initial state of the material the material being a polymer solution or dispersion
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00—Formation of filaments, threads, or the like
    • D01D5/0007—Electro-spinning
    • D01D5/0061—Electro-spinning characterised by the electro-spinning apparatus
    • D01D5/0069—Electro-spinning characterised by the electro-spinning apparatus characterised by the spinning section, e.g. capillary tube, protrusion or pin
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00—Formation of filaments, threads, or the like
    • D01D5/0007—Electro-spinning
    • D01D5/0061—Electro-spinning characterised by the electro-spinning apparatus
    • D01D5/0076—Electro-spinning characterised by the electro-spinning apparatus characterised by the collecting device, e.g. drum, wheel, endless belt, plate or grid
    • D01D5/0084—Coating by electro-spinning, i.e. the electro-spun fibres are not removed from the collecting device but remain integral with it, e.g. coating of prostheses
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00—Formation of filaments, threads, or the like
    • D01D5/0007—Electro-spinning
    • D01D5/0061—Electro-spinning characterised by the electro-spinning apparatus
    • D01D5/0092—Electro-spinning characterised by the electro-spinning apparatus characterised by the electrical field, e.g. combined with a magnetic fields, using biased or alternating fields
    • 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
    • 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
    • D01F6/54—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 polymers of unsaturated nitriles
    • 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
    • D04H1/42—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 characterised by the use of certain kinds of fibres insofar as this use has no preponderant influence on the consolidation of the fleece
    • D04H1/4382—Stretched reticular film fibres; Composite fibres; Mixed fibres; Ultrafine fibres; Fibres for artificial leather
    • D04H1/43838—Ultrafine fibres, e.g. microfibres
    • 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
    • D04H1/70—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres
    • D04H1/72—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres the fibres being randomly arranged
    • D04H1/728—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres the fibres being randomly arranged by electro-spinning
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M17/00—Producing multi-layer textile fabrics
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2307/00—Properties of the layers or laminate
    • B32B2307/70—Other properties
    • B32B2307/714—Inert, i.e. inert to chemical degradation, corrosion
    • B32B2307/7145—Rot proof, resistant to bacteria, mildew, mould, fungi
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
    • Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
    • Y02A50/30—Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change

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  • Engineering & Computer Science (AREA)
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  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Dispersion Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Chemical Or Physical Treatment Of Fibers (AREA)
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Abstract

The invention provides a plant-derived sunlight-driven efficient antibacterial antiviral multilayer composite nanofiber protective material prepared based on a high-voltage electrostatic spinning method and application thereof. The protective material is characterized in that a super-amphiphobic isolation layer, a high-efficiency degerming and disinfecting layer and a skin-friendly protective layer are sequentially arranged from outside to inside to replace the isolation layer in the common protective material. The invention can not only clear pathogens on the surface and efficiently filter particles, saliva, pathogens and the like absorbed in the air through the driving effect of the photocatalytic nano material and the synergistic effect of the plant extract, but also relieve adverse reactions caused by long-time use of the protective material and recycle the plant extract because the plant extract contains polyphenol and flavonoid active substances. The invention is particularly suitable for medical staff, infectious disease patients, people preventing virus infection and environments containing a large amount of or strong virus and bacteria.

Description

Plant-source sunlight-driven efficient antibacterial and antiviral multilayer composite nanofiber protective material and preparation method and application thereof
Technical Field
The invention belongs to the technical field of medical protective materials, and particularly relates to a plant-derived sunlight-driven efficient antibacterial and antiviral multilayer composite nanofiber protective material as well as a preparation method and application thereof.
Background
Since the new crown epidemic situation is generalized, more and more variant strains appear, the public health safety problem becomes more and more serious, and the medical protective material provides a protective measure for isolating germs for people. Although the common medical protective material isolates the transmission path of viruses and reduces the infection probability, some bacterial viruses are mainly transmitted by droplets and close contact, for example, the survival time of the new coronavirus in vitro is long, and the possibility of infection still exists under long-term touch contact. The common medical protective material has poor air permeability, causes adverse reactions such as chest distress and collapse caused by a large amount of sweating after long-term use, has short service life and poor recycling rate, and causes the problems of secondary infection, environmental pollution and the like because viruses are easy to adhere to the surface.
The amaranth is the only amaranth plant in China, is wind-sand resistant, drought resistant and salt and alkali resistant, can be used as a coast protection forest, and has good medicinal value. The research results show that the Chinese lobelia herb tablets can treat diseases such as headache, rheumatism, venereal disease, ulcer, herpes, pulmonary tuberculosis and the like, and some parts of the Chinese lobelia herb tablets can also be used as medicines for strengthening the body. The amaranth contains various chemical components with different structural types, wherein the content of flavonoid compounds is high, and the amaranth has antibacterial activity on staphylococcus aureus, escherichia coli, pseudomonas aeruginosa, candida albicans and other bacteria.
The commonly used inorganic antibacterial agent is mainly metal and compounds thereof, has the characteristics of contact antibacterial property, durability, water resistance, acid and alkali resistance, no harm to health and the like, for example, the contact reaction of silver ions and microorganisms can cause the common components of the microorganisms to be damaged or cause functional disorder. When a trace amount of silver ions reach the microbial cell membrane, the silver ions are charged with negative charges and are adsorbed and filtered firmly by virtue of Coulomb attraction, and the silver ions penetrate through the cell wall to enter the cell and react with sulfydryl, so that protein is solidified, the activity of cell synthetase is damaged, and the cell loses division and proliferation capacity and dies. Silver ions can also damage microbial electron transport systems, respiratory systems, and mass transport systems. g-C3N4Is an inorganic non-metallic photocatalyst for removing contaminants under visible light irradiation, the structure of which consists of carbon and nitrogen only, and which is stable under light irradiation in a solution of pH 0 to 14 due to strong covalent bonds between carbon and nitride atoms. g-C3N4The photocatalytic activity of (a) is relatively low due to poor absorption of visible light, slow electron/charge mobility, high electron-hole pair recombination and high surface inertness.
Disclosure of Invention
The invention aims to solve the technical problem of providing a plant-derived sunlight-driven efficient antibacterial and antiviral multilayer composite nanofiber protective material and a preparation method thereof, which can realize the purposes of high protective efficiency, good drug dispersibility, higher drug loading, environmental protection and obvious antiviral effect, and can be used for protective clothing and other protective tools to replace an isolation layer in a common protective material.
In order to solve the technical problems, the invention is realized by the following technical scheme:
a plant-derived sunlight-driven high-efficiency antibacterial and antiviral multilayer composite nanofiber protective material comprises a super-amphiphobic isolation layer, a high-efficiency degerming and disinfecting layer and a skin-friendly protective layer.
The super-amphiphobic isolation layer is a super-amphiphobic breathable fabric or non-woven fabric with a hydrophobic and oleophobic surface, and can be obtained by a commercially available method, so that the purpose is to reduce water vapor and splashed oil drops from entering the isolation material.
The efficient degerming and disinfecting layer is a nanofiber membrane material prepared from plant extracts, metal materials, photocatalysts and high-molecular polymers through high-voltage electrostatic spinning so as to kill entering pathogens (including viruses, bacteria, fungi and the like), and the electrostatic spinning composite solution is prepared by the following steps:
1) cold soaking dried powder of herba Ixeritis Sonchifoliae with organic solvent (preferably twice at room temperature for 14d and 7d respectively), filtering, and concentrating the filtrate to remove organic solvent to obtain herba Ixeritis Sonchifoliae extract;
2) placing a certain amount of nano photocatalyst and metal material in a light reaction tank, adding a proper amount of deionized water, uniformly stirring, reacting for 1-3h under the irradiation of a xenon lamp, and drying a solid phase after solid-liquid separation to obtain metal-loaded photocatalyst powder; the mass ratio of the nano photocatalyst to the metal material is preferably (19-99) to 1;
3) adding a certain amount of the polymer into a certain amount of the Ixeris amaranth extract, the metal-loaded photocatalyst powder and a certain amount of metal material, and adding a proper amount of surfactant (preferably Triton X-100, prevention of g-C3N4Powder agglomeration or precipitation), then adding a certain amount of unitary or binary solvent, and stirring until the high molecular polymer is completely dissolved to obtain a composite solution; the mass ratio of the used high molecular polymer, the Ixeris sonchifolia extract, the metal-loaded photocatalyst powder and the metal material is (6-12): (1-10): 1-5); the amount of the mono-or binary solvent used is such that the concentration of the high molecular weight polymer is 6 to 12% by weight.
Preferably, the organic solvent in the step 1) is one or more of absolute ethyl alcohol, methanol, acetone, acetic acid, ethyl acetate, chloroform and diethyl ether, or a mixed solution of the absolute ethyl alcohol, the methanol, the acetone, the acetic acid, the ethyl acetate, the chloroform and the diethyl ether and water; more preferably, it is 60% ethanol aqueous solution by volume.
Preferably, the nano photocatalyst in the step 2) is TiO2And derivatives thereof, ZnO and derivatives thereof, ZnS and derivatives thereof, Bi2WO6And derivatives thereof and g-C3N4And a derivative thereof.
Preferably, the skin-friendly protective layer is a fibrous membrane material woven by plant extracts of tannic acid and curcumin combined with a metal material through high-pressure electrostatic spinning, in order to reduce the damage of active free radicals generated by a photocatalyst to the skin, the electrostatic spinning composite solution comprises a certain proportion of high molecular polymer, curcumin, tannic acid, the metal material and a certain amount of monobasic or binary solvent, and is stirred until the high molecular polymer is completely dissolved; the mass ratio of the used high molecular polymer, curcumin, tannic acid and metal material is (8-12): 1-5): 0.1-1, and the dosage of the used monobasic or dibasic solvent is based on that the concentration of the high molecular polymer reaches 8-12 wt%.
Preferably, the metal material refers to one of Ag and a compound thereof, Cu and a compound thereof, and Zn and a compound thereof.
More preferably, the Ag compound comprises silver nitrate (AgNO)3) Silver carbonate (Ag)2CO3) Silver sulfate (Ag)2SO3) Silver chromate (Ag)2CrO4) (ii) a The Cu compound comprisesCopper sulfate (CuSO)4) Copper acetate ((CH)3COO)2Cu), copper oxide (CuO), cuprous oxide (Cu)2O), copper chloride (CuCl)2) Cuprous chloride (CuCl), copper nitrate (Cu (NO)3)2) Copper cyanide (Cu (CN))2) Copper fatty acid, copper naphthenate (C)22H14CuO4) (ii) a The Zn compound comprises zinc sulfate (ZnSO)4) Zinc chloride (ZnCl)2) Zinc nitrate (Zn (NO)3)2) Zinc hydroxide (Zn (OH)2）。
Preferably, the high molecular polymer is selected from one or more of the following: polylactic acid (PLA for short), polycaprolactone (PCL for short), polyvinylidene fluoride (PVDF for short), polyethylene glycol (PEG for short), polyurethane (PU for short), polyvinyl alcohol (PVA for short), polyvinyl butyral (PVB for short), polymethyl methacrylate (PMMA for short), polyacrylonitrile (PAN for short) and polyvinylpyrrolidone (PVP for short).
Preferably, the mono-or binary solvent is selected from one or more of: n, N-dimethylformamide, dichloromethane, chloroform, methanol, acetone, N-dimethylpropionamide, distilled water, and anhydrous ethanol.
Preferably, the parameters of electrospinning are: voltage: 12-25 kV, flow rate: 0.1-5 mL/h, receiving distance: 10-20 cm, jet needle: number 15-24, drum speed: 0.1-10 m/min; more preferably: voltage: 17 kV, flow rate: 1.0 mL/h, reception distance: 15 cm, jet needle: no. 20, drum rotation speed: 0.5 m/min.
The invention discloses a preparation method of a plant-source sunlight-driven efficient antibacterial antiviral multilayer composite nanofiber protective material, which comprises the following steps: and compounding the super-amphiphobic isolation layer, the high-efficiency degerming and disinfecting layer and the skin-friendly protective layer by a high-voltage electrostatic spinning process in sequence to obtain the composite material.
Compared with the prior art, the invention has the following beneficial technical effects:
(1) the invention provides a plant-derived sunlight-driven efficient antibacterial and antiviral multilayer composite nanofiber protective material prepared based on a high-voltage electrostatic spinning method, which replaces an isolation layer in a common protective material, is stable in structure, uniform in particle size and good in dispersity, can maintain the efficient antibacterial and bacteriostatic performance of a medicament, and has high filtering efficiency.
(2) The preparation method related to the method is simple to operate, can be used for rapid mass production, is nontoxic and pollution-free, has good repeatability and firm adhesion, does not need to add any chemical adhesive, hot adhesive and bonding agent, has mild reaction product and is environment-friendly.
(3) The added medicines can realize nano preparation, the smaller particle size can improve the loading capacity of the medicines, and the use amount of the antibacterial medicines is reduced, so that the influence on the drug resistance of bacteria is reduced.
(4) The composite electrostatic spinning nanofiber protective material prepared by the method carries electrostatic charges, has an electrostatic attraction effect on particles, pathogens and the like, is strong in attraction force, high in filtering efficiency, capable of efficiently filtering particles, saliva, pathogens and the like absorbed into air, convenient and fast, good in charge stability, not easy to decompose and discolor, and does not have a chemical reaction with other components.
(5) The amaranth, the tannic acid and the curcumin which are used in the method are natural products with wide sources, are green and environment-friendly, have no toxicity or pollution, contain a large amount of flavonoid compounds and a plurality of trace metals, and have an inhibiting effect on a plurality of viruses and bacteria; tannic acid structurally has a large number of hydroxyl groups, and a small number of tannic acid can remove various free radicals, protect skin and the like, and prevent adverse effects on human bodies.
Drawings
To further clarify the advantages and objects of the solution according to the present invention, reference will now be made in brief to the accompanying drawings which illustrate an example or related art in the description.
FIG. 1 is an SEM electron micrograph of the composite nanofiber protective material obtained in the present invention;
FIG. 2 is a TEM image of the composite nanofiber protective material obtained by the present invention;
FIG. 3 is a structural simulation diagram of the composite nanofiber protective material obtained by the present invention;
FIG. 4 is a graph showing the in vitro Escherichia coli colony antibacterial results of the composite nanofiber protective material and a commercial mask according to the present invention;
FIG. 5 is a graph showing the antibacterial results of the composite nanofiber protective material obtained in the present invention at different times;
FIG. 6 is a graph showing the antibacterial effect of the composite nanofiber protective material obtained in the present invention on Staphylococcus aureus under different contents of photocatalysts;
FIG. 7 is a diagram of the photocatalytic mechanism of the composite nanofiber protective material obtained by the present invention;
FIG. 8 is a graph showing the results of photodegradation of methylene blue MB by the composite nanofiber protective material obtained in the present invention;
fig. 9 is a simulation diagram of the results of photodegradation of methylene blue MB by the composite nanofiber protective material obtained in the present invention.
Detailed Description
The invention will be further described with reference to the following figures and examples, but the embodiments of the invention are not limited thereto.
Example 1
(1) Weighing 1g PAN powder, adding 8.5 g DMF, magnetically stirring at 50 deg.C for 30min, adding 0.1 g Tannic Acid (TA), 0.3 g curcumin (Cur) and 0.1 g AgNO respectively3Magnetically stirring for 3h to obtain PAN/TA/Cur/Ag precursor solution;
(2) weighing 50 g of Ixeris sonchifolia, drying in shade for 7d, removing surface water, drying at 50 deg.C for 10h, pulverizing, soaking the powder twice (14 d, 7 d) with 60% ethanol water solution at normal temperature, filtering, mixing filtrates, distilling under reduced pressure (rotary evaporator RE-2000A, Shanghai subsume Biochemical apparatus factory) to obtain Ixeris sonchifolia extract, and storing at low temperature;
(3) 0.97g g-C3N4And 0.03 g AgNO3Adding into a light reaction tank, adding 50 mL deionized water, stirring, placing under xenon lamp (PLS-SXE 300D, Beijing Bofei technology Co., Ltd.) for irradiation, 2 hr, vacuum filtering, and drying at 50 deg.C for 10 hr to obtain metal-loaded photocatalyst powder Ag/g-C3N4For standby;
(4) 1g PAN powder was weighed and added0.5 g of the extract of Trifolium Pratentis obtained in step (2), and 0.1 g of the photocatalyst powder Ag/g-C loaded with metal obtained in step (3)3N4And 0.3 g AgNO35 drops of surfactant Triton X-100 were added to prevent g-C3N4The powder was agglomerated and precipitated, and finally 8.1 g DMF was added and stirred until the polymer was completely dissolved to give PAN/M3N4Compounding the precursor solution for later use;
(5) firstly, taking a non-woven fabric made of PP (polypropylene) as a bottom layer, secondly, taking a PAN/TA/Cur/Ag fiber membrane as a middle layer, and spinning the PAN/TA/Cur/Ag precursor solution by a high-voltage electrostatic spinning machine, wherein the dosage is 3 mL, and the voltage is as follows: 16 kV, flow rate: 1.5 ml/h, receiving distance: 12 cm, jet needle: no. 20, drum rotation speed: 0.5 m/min; finally, using PAN/M3N4The fiber membrane is the upper layer and is spun by a high-voltage electrostatic spinning machine into PAN/M3N4Precursor solution, dosage 5 mL, voltage: 18 kV, flow rate: 1.0 ml/h, receiving distance: 10 cm, jet needle: no. 20, drum rotation speed: 0.5 m/min. After spinning, the composite fiber membrane is dried for 6 hours at the temperature of 45 ℃ to obtain the composite nanofiber protective material.
Example 2
(1) Weighing 1g PAN powder, adding 8.3 g DMF, magnetically stirring at 50 deg.C for 30min, adding 0.3 g Tannic Acid (TA), 0.3 g curcumin (Cur) and 0.1 g AgNO respectively3Magnetically stirring for 3h to obtain PAN/TA/Cur/Ag precursor solution;
(2) weighing 50 g of Ixeris sonchifolia, drying in shade for 7d, removing surface water, drying at 50 deg.C for 10h, pulverizing, soaking the powder twice (14 d, 7 d) with 60% ethanol water solution at normal temperature, filtering, mixing filtrates, distilling under reduced pressure (rotary evaporator RE-2000A, Shanghai subsume Biochemical apparatus factory) to obtain Ixeris sonchifolia extract, and storing at low temperature;
(3) 0.97g g-C3N4And 0.03 gAgNO3Adding into a light reaction tank, adding 50 mL deionized water solution, stirring, placing under xenon lamp (PLS-SXE 300D, Beijing Bofei technology Co., Ltd.) for irradiating for 2 hr, vacuum filtering, and drying at 50 deg.C for 10 hr to obtain metal-loaded photocatalyst powder Ag/g-C3N4For standby;
(4) weighing 1g PAN powder, and adding 0.5 g of the extract of Ixeris amaranus obtained in step (2), 0.1 g of the metal-supporting photocatalyst powder Ag/g-C obtained in step (3)3N4And 0.5 g AgNO35 drops of surfactant Triton X-100 were added to prevent g-C3N4The powder was agglomerated and precipitated, and finally 7.9 g of DMF was added and stirred until the polymer was completely dissolved, to give PAN/M3N4Compounding the precursor solution for later use;
(5) firstly, using a super-amphiphobic breathable fabric as a bottom layer; secondly, using the PAN/TA/Cur/Ag fiber membrane as a middle layer, spinning the PAN/TA/Cur/Ag precursor solution through a high-voltage electrostatic spinning machine, wherein the dosage is 3 mL, and the voltage is as follows: 16 kV, flow rate: 1.5 ml/h, receiving distance: 12 cm, jet needle: no. 20, drum rotation speed: 0.5 m/min; finally, using PAN/M3N4The fiber membrane is the upper layer and is spun by a high-voltage electrostatic spinning machine into PAN/M3N4Precursor solution, dosage 5 mL, voltage: 18 kV, flow rate: 1.0 ml/h, receiving distance: 10 cm, jet needle: no. 20, drum rotation speed: 0.5 m/min. After spinning, the composite fiber membrane is dried for 6 hours at the temperature of 45 ℃ to obtain the composite nanofiber protective material.
Example 3
(1) Weighing 1g PAN powder, adding 8.1 g DMF, magnetically stirring at 50 deg.C for 30min, adding 0.5 g Tannic Acid (TA), 0.3 g curcumin (Cur) and 0.1 g AgNO respectively3Magnetically stirring for 3h to obtain PAN/TA/Cur/Ag precursor solution;
(2) weighing 50 g of Ixeris sonchifolia, drying in shade for 7d, removing surface water, drying at 50 deg.C for 10h, pulverizing, soaking the powder twice (14 d, 7 d) with 60% ethanol water solution at normal temperature, filtering, mixing filtrates, distilling under reduced pressure (rotary evaporator RE-2000A, Shanghai subsume Biochemical apparatus factory) to obtain Ixeris sonchifolia extract, and storing at low temperature;
(3) 0.97g g-C3N4And 0.05 gAgNO3Adding into a light reaction tank, adding 50 mL deionized water solution, stirring, and placing into a xenon lamp (PLS-SXE 300D, Beijing Bofei)From science and technology Co., Ltd.), 2h, vacuum filtration, drying at 50 ℃ for 10h to obtain the metal-loaded photocatalyst powder Ag/g-C3N4For standby;
(4) weighing 1g PAN powder, and adding 0.5 g of the extract of Ixeris amaranus obtained in step (2), 0.5 g of the metal-supporting photocatalyst powder Ag/g-C obtained in step (3)3N4And 0.5 g AgNO35 drops of surfactant Triton X-100 were added to prevent g-C3N4Agglomerating and precipitating the powder, finally adding 7.5 g of DMF, and stirring until the polymer is completely dissolved to obtain PAN/M3N4Compounding the precursor solution for later use;
(5) firstly, using a super-amphiphobic breathable fabric as a bottom layer; secondly, using the PAN/TA/Cur/Ag fiber membrane as a middle layer, spinning the PAN/TA/Cur/Ag precursor solution through a high-voltage electrostatic spinning machine, wherein the dosage is 3 mL, and the voltage is as follows: 16 kV, flow rate: 1.5 ml/h, receiving distance: 12 cm, jet needle: no. 20, drum rotation speed: 0.5 m/min; finally, using PAN/M3N4The fiber membrane is the upper layer and is spun by a high-voltage electrostatic spinning machine into PAN/M3N4Precursor solution, dosage 5 mL, voltage: 18 kV, flow rate: 1.0 ml/h, receiving distance: 10 cm, jet needle: no. 20, drum rotation speed: 0.5 m/min. After spinning, the composite fiber membrane is dried for 6 hours at 50 ℃ to obtain the composite nanofiber protective material.
Example 4
(1) Weighing 1g PAN powder, adding 8.1 g DMF, magnetically stirring at 50 deg.C for 30min, adding 0.5 g Tannic Acid (TA), 0.3 g curcumin (Cur) and 0.1 g AgNO respectively3Magnetically stirring for 3h to obtain PAN/TA/Cur/Ag precursor solution;
(2) weighing 50 g of Ixeris sonchifolia, drying in shade for 7d, removing surface water, drying at 50 deg.C for 10h, pulverizing, soaking the powder twice (14 d, 7 d) with 60% ethanol water solution at normal temperature, filtering, mixing filtrates, distilling under reduced pressure (rotary evaporator RE-2000A, Shanghai subsume Biochemical apparatus factory) to obtain Ixeris sonchifolia extract, and storing at low temperature;
(3) 0.97g g-C3N4And 0.05 gAgNO3Adding into a light reaction tank, adding 50 mL deionized water solution, stirring, placing under xenon lamp (PLS-SXE 300D, Beijing Bofei technology Co., Ltd.) for irradiation, 2 hr, vacuum filtering, and drying at 50 deg.C for 10 hr to obtain metal-loaded photocatalyst powder Ag/g-C3N4For standby;
(4) weighing 1g PAN powder, and adding 0.5 g of the extract of Ixeris amaranus obtained in step (2), 0.1 g of the metal-supporting photocatalyst powder Ag/g-C obtained in step (3)3N4And 0.5 g AgNO35 drops of surfactant Triton X-100 were added to prevent g-C3N4The powder was agglomerated and precipitated, and finally 7.9 g of DMF was added and stirred until the polymer was completely dissolved, to give PAN/M3N4Compounding the precursor solution for later use;
(5) firstly, using a super-amphiphobic breathable fabric as a bottom layer; secondly, using the PAN/TA/Cur/Ag fiber membrane as a middle layer, spinning the PAN/TA/Cur/Ag precursor solution through a high-voltage electrostatic spinning machine, wherein the dosage is 3 mL, and the voltage is as follows: 16 kV, flow rate: 1.5 ml/h, receiving distance: 12 cm, jet needle: no. 20, drum rotation speed: 0.5 m/min; finally, using PAN/M3N4The fiber membrane is the upper layer and is spun by a high-voltage electrostatic spinning machine into PAN/M3N4Precursor solution, dosage 5 mL, voltage: 18 kV, flow rate: 1.0 ml/h, receiving distance: 10 cm, jet needle: no. 20, drum rotation speed: 0.5 m/min. After spinning, the composite fiber membrane is dried for 6 hours at 50 ℃ to obtain the composite nanofiber protective material.
The above embodiments are preferred embodiments of the present invention, however, the present invention is not limited thereto, and various modifications and substitutions of equivalent forms of the present invention should be made within the scope of the present invention.
Test method
The scanning electron microscope image of the composite nanofiber protective material obtained in example 1 of the present invention is shown in fig. 1. In fig. 1, the magnification is 10000 times. As can be seen from figure 1, the obtained composite nanofiber protective material has smooth surface and no beads, and the fibers are mutually crosslinked to form a porous structure, so that pathogens in the air can be effectively intercepted.
The transmission electron microscope image of the composite nanofiber protective material obtained in example 1 of the present invention is shown in fig. 2. As can be seen from FIG. 2, silver and carbon nitride have been successfully incorporated into the fibers and have a large amount of Ag/g-C on the surface3N4The nano particles increase the contact area with pollutants and pathogens, thereby effectively improving the photocatalytic capacity and the antibacterial capacity of the nano particles, and enabling the nano particles to have higher degradation rate, higher degradation efficiency and higher antibacterial rate.
The structure simulation diagram of the composite nanofiber protective material obtained in the embodiment 1 of the present invention is shown in fig. 3. Therefore, each layer of material can be tightly combined together through electrostatic attraction and the adhesion force of the polymer by the high-voltage electrostatic spinning method without adding any chemical adhesive, thermal adhesive and bonding agent.
The in vitro escherichia coli colony antibacterial result of the composite nanofiber protective material obtained in the embodiment 1 of the invention and the commercial mask is shown in fig. 4. And (3) detecting according to the steps 3 and 4 in the national standard GB/T30706-2014 of the people's republic of China, and respectively putting each sample into a clean plate with the test surface facing upwards. 0.2mL of the prepared inoculum was accurately measured with a pipette and dropped onto the surface of each sample, carefully covered with a thin film, and the film was adjusted to disperse the inoculum evenly. The xenon lamp (PLS-SXE 300D, Beijing Bo Fei Shi Tech Co., Ltd.) was turned on and stabilized for 0.5 h or more, then the height or power of the fluorescent lamp was adjusted to adjust the intensity of light to 7500 Lux, and 3 blanks and 3 photocatalytic samples were placed under light conditions, and the other 3 blanks and 3 photocatalytic samples were placed under dark conditions.
Antibacterial ratio RGeneral assemblyThe values are calculated in percent, according to equation (1):
R general assembly =（C 0 -C 1 )/C 0 ×100 （1）
In the formula:
C0-clear conditionCounting the viable bacteria of the lower control sample after culture;
C1and counting the viable bacteria CFU of the photo-catalytic sample after culture under the bright condition.
The antibacterial value R of the photocatalytic material under the irradiation of a fluorescent lamp is calculated in percentage according to the formula (2):
R light (es) =（B 1 -C 1 )/B 1 ×100 （2）
In the formula:
B1and counting the viable bacteria CFU of the photo-catalytic sample after culture under dark conditions.
The in-vitro escherichia coli colony antibacterial result of the composite nanofiber protective material obtained in the embodiment 1 of the invention is increased along with the change of illumination time. In a dark environment, compared with a commercial mask, the antibacterial rate of the composite nanofiber protective material obtained by the invention reaches 30-40%; after the composite nanofiber protective material is illuminated for 3 hours, the antibacterial rate of the composite nanofiber protective material obtained by the invention reaches 90% -95%, and the composite nanofiber protective material obtained by the invention has excellent photocatalytic antibacterial capability. With the increase of the illumination time, the antibacterial result of the composite nanofiber protective material obtained by the invention is improved, as shown in figure 5. After the cyclic illumination is carried out for 1 hour, 2 hours and 3 hours, the antibacterial rates of the composite nanofiber protective material obtained by the invention respectively reach 76.97 +/-0.71%, 88.58 +/-2.80% and 98.65 +/-1.49%, and the result shows that the composite nanofiber protective material obtained by the invention has the capability of recycling. The influence of the content of the photocatalyst on the antibacterial result of the composite nanofiber protective material obtained by the invention is studied at the same time, and is shown in fig. 6. With the increase of the content of the photocatalyst, the antibacterial rate of the composite nanofiber protective material obtained by the invention is increased, and when the content of the photocatalyst is 3wt%, the antibacterial rate reaches 96.73%; when the content of the photocatalyst is 5wt%, the antibacterial rate reaches 97.47%; when the content of the photocatalyst is 7wt%, the antibacterial rate is close to 100%. The composite nanofiber protective material obtained by the invention has the advantages of low usage amount and resource saving.
The photocatalytic principle of the composite nanofiber protective material obtained by the invention under illumination is shown in fig. 7. When the composite nanofiber protective material obtained by the invention is irradiated by sunlight, the photon energy is higher than g-C3N4Band gap (2.7 eV) of (a), wherein electrons (e)-) Transfer from Valence Band (VB) to Conduction Band (CB) while leaving the same number of photogenerated holes (h) in VB+). The photo-excited electrons may be from g-C3N4Transfer to Ag with a CB to g-C ratio of Ag3N4Is narrow. In Ag or g-C3N4The electrons accumulated in the CB can be transferred to the oxygen molecules adsorbed on the surface to form O2Radicals such as HOO, OH and the like, and photo-excited holes react with surface-bound water molecules to generate OH radicals. The large amount of reactive oxidizing species generated can react with surrounding dyes and other contacts or enter the interior of the pathogen, destroy protein function and DNA, destroy bacterial cell membranes, cause the death of the pathogen and produce antibacterial and antiviral effects.
In order to evaluate the photocatalytic degradation performance of the composite nanofiber protective material obtained by the invention, methylene blue (molecular weight: 319.85) dye without azo is selected for testing. Preparing a methylene blue dye into 100mL of solution with the concentration of 10mg/L, adding the composite nanofiber protective material prepared in the embodiment 1 of the invention with the size of 2 cm multiplied by 2 cm into the methylene blue solution, fully stirring the solution in a dark place until the adsorption-desorption balance is achieved, placing an ultraviolet lamp above the liquid level of the solution for irradiation, sampling and centrifuging at intervals, taking a supernatant, measuring the absorbance of the solution by using a spectrophotometer, and calculating the degradation rate eta; the calculation formula of the degradation rate eta is as follows:
η (%) = (C0-Ct)/C0 ×100 (3)
ln(Ct/C0) = kt (4)
in the formula, C0Initial absorbance of the dye solution, CtIs the absorption of the dye solution after a time tAnd (4) degree.
The time-dependent change curve of the degradation rate of the composite nanofiber protective material obtained by the invention in the methylene blue dye solution is shown in FIG. 8, and ln (C) in the methylene blue dye solution0/Ct) The time profile is shown in FIG. 9. As can be seen from fig. 8 and 9, the composite nanofiber protective material in embodiment 1 of the present invention has a good degradation effect on methylene blue dye, the degradation time on the dye is within 150min, the degradation rates are all up to 95%, the overall degradation rate is high, the degradation efficiency is high, and the requirements of practical applications can be met.
In order to evaluate the filtration performance test of the composite nanofiber protective material obtained by the invention, detection is carried out according to the step 6.3 in the national standard GB 2626-plus 2019 of the people's republic of China, and the filtration efficiency and the gas flow of a NaCl particulate matter detection sample are as follows: 85L/min, NaCl particulate matter concentration: 20mg/m3Temperature: 21.3 ℃, relative humidity: 36 percent. After the composite nanofiber protective material obtained by the invention is subjected to a loading test, the filtering efficiency of NaCl particles reaches 99.801%, 99.839% and 99.822%, and the standard of a KN95 mask is reached; after a loading test is not carried out, the filtering efficiency of NaCl particles reaches 99.989%, 99.958% and 99.968%, and reaches the standard of a KN100 mask, which shows that the composite nanofiber protective material obtained by the invention has excellent filtering efficiency and can meet the requirements of practical application.
Table 1 filtration performance test results of the composite nanofiber protective material of the present invention
Figure 257057DEST_PATH_IMAGE002
。

Claims (10)

1. A plant-derived sunlight-driven efficient antibacterial and antiviral multilayer composite nanofiber protective material is characterized in that: comprises a super-amphiphobic isolation layer, a high-efficiency degerming and disinfecting layer and a skin-friendly protective layer;
the efficient degerming and disinfecting layer is a nanofiber membrane material prepared by high-voltage electrostatic spinning, and the electrostatic spinning composite solution is prepared by the following steps:
cold soaking dried powder of herba Ixeritis Sonchifoliae with organic solvent, filtering, and concentrating the filtrate to remove organic solvent to obtain herba Ixeritis Sonchifoliae extract;
placing a certain amount of nano photocatalyst and metal material in a light reaction tank, adding a proper amount of deionized water, uniformly stirring, reacting for 1-3h under the irradiation of a xenon lamp, and drying a solid phase after solid-liquid separation to obtain metal-loaded photocatalyst powder; the mass ratio of the nano photocatalyst to the metal material is preferably (19-99) to 1;
taking a certain amount of high molecular polymer, adding a certain amount of the Ixeris amaranth extract, the metal-loaded photocatalyst powder and a certain amount of metal material, adding a proper amount of surfactant, adding a certain amount of unitary or binary solvent, and stirring until the high molecular polymer is completely dissolved to obtain a composite solution; the mass ratio of the used high molecular polymer, the Ixeris sonchifolia extract, the metal-loaded photocatalyst powder and the metal material is (6-12): (1-10): 1-5); the amount of the mono-or binary solvent used is such that the concentration of the high molecular weight polymer is 6 to 12% by weight.
2. The multilayer composite nanofiber shield material according to claim 1, wherein: the organic solvent in the step 1) is one or more of absolute ethyl alcohol, methanol, acetone, acetic acid, ethyl acetate, chloroform and ether, or a mixed solution of the absolute ethyl alcohol, the methanol, the acetone, the acetic acid, the ethyl acetate, the chloroform and the ether and water; step 2) the nano photocatalyst is TiO2And derivatives thereof, ZnO and derivatives thereof, ZnS and derivatives thereof, Bi2WO6And derivatives thereof and g-C3N4And a derivative thereof.
3. The multilayer composite nanofiber shield material according to claim 1, wherein: the skin-friendly protective layer is a fiber membrane material woven by high-pressure electrostatic spinning, and the electrostatic spinning composite solution comprises a high molecular polymer, curcumin, tannic acid, a metal material and a certain amount of a unitary or binary solvent in a certain proportion, and is stirred until the high molecular polymer is completely dissolved; the mass ratio of the used high molecular polymer, curcumin, tannic acid and metal material is (8-12): 1-5): 0.1-1, and the dosage of the used monobasic or dibasic solvent is based on that the concentration of the high molecular polymer reaches 8-12 wt%.
4. The multilayer composite nanofiber shield as claimed in claim 3, wherein: the metal material refers to one of Ag and a compound thereof, Cu and a compound thereof, and Zn and a compound thereof.
5. The multilayer composite nanofiber shield as claimed in claim 3, wherein: the Ag compound comprises silver nitrate, silver carbonate, silver sulfate and silver chromate; the Cu compound comprises copper sulfate, copper acetate, copper oxide, cuprous oxide, copper chloride, cuprous chloride, copper nitrate, copper cyanide, fatty acid copper and copper naphthenate; zn compounds include zinc sulfate, zinc chloride, zinc nitrate, and zinc hydroxide.
6. The multilayer composite nanofiber shield as claimed in claim 3, wherein: the high molecular polymer is selected from one or more of the following: polylactic acid, polycaprolactone, polyvinylidene fluoride, polyethylene glycol, polyurethane, polyvinyl alcohol, polyvinyl butyral, polymethyl methacrylate, polyacrylonitrile and polyvinylpyrrolidone.
7. The multilayer composite nanofiber shield as claimed in claim 3, wherein: the mono-or binary solvent is selected from one or more of the following: n, N-dimethylformamide, dichloromethane, chloroform, methanol, acetone, N-dimethylpropionamide, distilled water, and anhydrous ethanol.
8. The multilayer composite nanofiber shield as claimed in claim 3, wherein: the parameters of electrostatic spinning are as follows: voltage: 12-25 kV, flow rate: 0.1-5 mL/h, receiving distance: 10-20 cm, jet needle: number 15-24, drum speed: 0.1-10 m/min; more preferably: voltage: 17 kV, flow rate: 1.0 mL/h, reception distance: 15 cm, jet needle: no. 20, drum rotation speed: 0.5 m/min.
9. The preparation method of the plant-derived sunlight-driven efficient antibacterial and antiviral multilayer composite nanofiber protective material as claimed in any one of claims 1 to 8, is characterized by comprising the following steps: and compounding the super-amphiphobic isolation layer, the high-efficiency degerming and disinfecting layer and the skin-friendly protective layer by a high-voltage electrostatic spinning process in sequence to obtain the composite material.
10. Use of the plant-derived sun-driven highly effective antibacterial and antiviral multi-layer composite nanofiber protective material as claimed in any one of claims 1 to 8 in protective clothing and other protective gear.
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Publication number Priority date Publication date Assignee Title
CN101897347A (en) * 2010-07-09 2010-12-01 华南农业大学 Plant-based bacteriostat, preparation method thereof and application thereof
CN107497182A (en) * 2017-08-17 2017-12-22 东华大学 A kind of composite nano fiber filtering material for having photocatalysis/antibacterial functions concurrently and preparation method thereof
CN111184026A (en) * 2020-03-05 2020-05-22 上海纳米技术及应用国家工程研究中心有限公司 Preparation method of nano-copper/bismuth vanadate composite antibacterial agent
CN112107046A (en) * 2020-10-30 2020-12-22 湖南大学 Mask based on electrostatic adsorption filtration and preparation method thereof

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101897347A (en) * 2010-07-09 2010-12-01 华南农业大学 Plant-based bacteriostat, preparation method thereof and application thereof
CN107497182A (en) * 2017-08-17 2017-12-22 东华大学 A kind of composite nano fiber filtering material for having photocatalysis/antibacterial functions concurrently and preparation method thereof
CN111184026A (en) * 2020-03-05 2020-05-22 上海纳米技术及应用国家工程研究中心有限公司 Preparation method of nano-copper/bismuth vanadate composite antibacterial agent
CN112107046A (en) * 2020-10-30 2020-12-22 湖南大学 Mask based on electrostatic adsorption filtration and preparation method thereof

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