CN115787282A - Two-dimensional alkene modified antiviral photo-thermal nanofiber and preparation method thereof - Google Patents
Two-dimensional alkene modified antiviral photo-thermal nanofiber and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a two-dimensional alkene modified antiviral photo-thermal nanofiber and a preparation method thereof, wherein the preparation method comprises the following steps: preparing a layered two-dimensional alkene nanosheet by adopting an inorganic acid etching or solvothermal method; and loading the two-dimensional alkene nano-sheets on the non-woven nano-fibers to prepare the anti-virus non-woven material. Due to the excellent photo-thermal effect of the two-dimensional alkene, the antiviral nanofiber prepared by the method has a good antiviral effect on various viruses under the condition of simulating sunlight, and the antiviral activity on new coronavirus is more than 99.9%. Therefore, the photothermal antiviral nanofiber prepared by the method can be used as a functional non-woven material and is suitable for antiviral protection in various scenes.
Description
Technical Field
The invention relates to a preparation method of two-dimensional alkene modified antiviral photo-thermal nano-fibers, belonging to the technical field of preparation of antiviral functional materials and biomedical protective materials.
Background
The antibacterial and antiviral fabric plays an important role in the field of medical health, can effectively block the spread of viruses and provides effective protection for the life health of human bodies. Since the pneumonia caused by the novel coronavirus is prevalent in 2019, protective materials represented by antiviral fabrics, such as medical surgical masks, N95 masks, protective clothing and the like, have entered the daily life of residents from the medical and health industry and become an essential part of citizens in outgoing, so that the diffusion and the propagation of the virus are effectively blocked, and the life health of people is guaranteed. Because the fiber diameter and the mesh of the non-woven fabric can be controlled within extremely small values, the filtering effect on viruses and bacteria is far better than that of a woven fabric, and the anti-virus fabric is mainly a non-woven fabric at present, and particularly a fabric filtering layer represented by polypropylene melt-blown cloth.
However, although most of viruses and bacteria can be effectively filtered by controlling the fiber diameter and the mesh density of the nonwoven fabric, the nonwoven fabric itself has no capability of killing bacteria and viruses, and the bacteria and viruses remained on the surface of the nonwoven fabric after the protective material is used have a great threat to environmental pollution and secondary spreading of viruses. At present, researchers improve the antiviral capacity of non-woven fabrics by introducing antiviral agents, and endow the non-woven fabrics with the function of killing viruses under the condition of meeting specific conditions. CN113737519A adds metal nano-wires and antibacterial polypeptide as antiviral slurry in the process of fabric forming process, so as to realize antiviral activity of more than 96% to new coronavirus, influenza A virus and the like; CN113564928A adopts modified guanidino polymer as organic antibacterial agent, neomycin sulfate as antibiotic, endows the mask with long-acting antibacterial and antiviral functions, and solves the problem of leaching effect of metal nanoparticle modified mask; CN113576076A, CN113576077A, CN216089007U and CN115142194A improve the antiviral ability of the nonwoven fabric by thus using graphene as an antiviral agent. The two-dimensional alkene material has excellent photo-thermal conversion capability, so that the two-dimensional alkene material can be used as an antiviral agent to realize the photo-thermal antiviral function of the non-woven fabric. The antiviral ability of the non-woven material is effectively improved by introducing the two-dimensional alkene material, the antiviral activity of the antiviral non-woven fabric prepared by the method is more than 99.9 percent on new coronavirus, and the method has important significance on the practical application of the photothermal antiviral non-woven fabric in the field of medical health.
Disclosure of Invention
The invention aims to provide two-dimensional alkene modified antiviral photo-thermal nano-fiber and a preparation method thereof.
1. Inorganic acid etching method for synthesizing layered two-dimensional olefin nano-sheet (MXene)
Slowly adding MAX phase raw materials into hydrofluoric acid solution, and magnetically stirring and reacting for 12-72 h at 30-50 ℃; centrifuging the reacted solution at 3000-5000 rpm for 15-35 min; then collecting the centrifuged precipitate, dispersing the precipitate in deionized water again, and performing vacuum drying after suction filtration to obtain etched multilayer MXene powder; taking the multilayer MXene powder obtained in the step, and preparing the multilayer MXene powder into a solution with the concentration of 1-5 mg mL -1 Centrifuging the water solution at 5000-8000 rpm for 20-35 min; centrifuging the centrifuged supernatant for 20-40 min at 15000-20000 rpm, collecting the centrifuged precipitate, and vacuum drying at 40-60 deg.C overnight to obtain MXene powder with less layers.
Wherein, the MAX phase raw material is Ti 3 AlC 2 、Ti 2 AlC、Ti 3 AlCN、V 2 AlC、V 3 AlC 2 、V 3 AlCN、Nb 3 AlC 2 、Nb 2 AlC、Nb 3 AlCN、Mo 2 AlC、Cr 2 AlC、Hf 2 One or more AlC with the concentration of 0.05-0.5 g mL in hydrofluoric acid solution -1 。
2. Solvothermal method for synthesizing layered two-dimensional alkene nanosheet
Dispersing a source material in a solvent at a certain concentration (0.01-0.1 mmol/mL) by adopting a solvothermal method, and magnetically stirring for 5-20 min; after being mixed evenly, the mixture is subjected to solvothermal reaction for 0.1 to 720min at a temperature of between 50 and 210 ℃; and after the reaction is finished, cooling to room temperature, centrifuging at 5000-18000 rpm, and drying in vacuum at 40-100 ℃ to obtain the required layered two-dimensional alkene nanosheet.
The source material is raw materials required for preparing graphene, silylene, germanium alkene, tin alkene, tellurium alkene and boron alkene, and comprises one or two of a carbon source, a silicon source, a germanium source, a tin source, a tellurium source and a boron source.
The solvent is one or two of ethanol, ethyl acetate, isopropanol, n-butanol, tert-butanol, toluene, n-hexane, petroleum ether, dichloromethane and deionized water.
3. Preparation of polymer nanofibers by non-woven technology
The polymer nano-fiber is prepared by adopting a non-woven process, which comprises one or two of a spun-bonded non-woven technology, a melt-blown non-woven technology, a spun-bonded melt-blown (SMS) composite non-woven technology, a wet non-woven technology, a spunlace non-woven technology, a needle-punched non-manufacturing technology, a thermal bonding non-woven technology and a pulp air-laid non-woven technology.
The nano-fibers comprise one or two or three of polymers such as polypropylene, polyethylene, polyester fibers, polylactic acid, levorotatory polylactic acid, dextrorotatory polylactic acid, cellulose acetate, regenerated cellulose, polycarbonate, polyacrylonitrile, nylon fibers, polycaprolactone, polyethylene oxide, polyethylene glycol terephthalate, polyamide, polyimide, polystyrene, polyurethane, polyvinyl alcohol, polyvinylidene fluoride, collagen, chitosan, fibroin and the like.
4. Preparation of two-dimensional alkene loaded antiviral photo-thermal nano-fiber
The preparation method of the two-dimensional alkene-loaded nanofiber comprises in-situ treatment and post-treatment.
The in-situ treatment is to mix the precursor solution of the two-dimensional alkene and the nanofiber and then prepare the mixture by a non-woven technology; and the post-treatment is to load the two-dimensional olefin nano-sheets on the non-woven nano-fibers in the modes of spraying, dip coating, spin coating, dipping-pulling, brush coating and the like.
The mass ratio of the layered two-dimensional olefin nano-sheets to the non-woven nano-fibers is 0-0.5.
5. Antiviral testing
Using ISO 21702:2019, the method of the invention is used for evaluating the antiviral performance of the photo-thermal nano-fiber prepared by the invention.
The invention also provides application of the antiviral photothermal nano fiber prepared by the preparation method in the aspect of antiviral activity of the novel coronavirus. The antivirus photothermal nanofiber has excellent photothermal effect under the illumination condition, can effectively convert light energy into heat energy through high-efficiency photothermal conversion capacity, kills viruses attached to the surface of the fiber fabric material, improves the antivirus activity of the fiber fabric material, prolongs the service cycle of the antivirus fabric, reduces resource waste and environmental pollution caused by disposable protective materials, and ensures the life health of human beings.
In conclusion, compared with the prior art, the two-dimensional alkene modified antiviral photothermal nanofiber prepared by the invention has the following advantages:
1. the antiviral nanofiber prepared by the invention greatly improves the antiviral ability of the medical non-woven material by utilizing the excellent photo-thermal conversion ability of the two-dimensional vinyl material, and has the characteristics of higher controllability and flexibility of the antiviral ability and remote accurate control due to the remote control ability of the photo-thermal effect and the universality of a light source.
2. The two-dimensional alkene loaded photo-thermal nanofiber prepared by the invention has the antiviral activity of more than 99.9% on new coronavirus.
Drawings
FIG. 1 shows the photo-thermal polypropylene melt-blown fabric loaded with SnS nanosheets and the unsupported polypropylene melt-blown fabric prepared in example 1The antiviral ability of the product changes with the change of illumination time, and the optical density is 85mW cm -2 。
Detailed Description
The preparation method and properties of the two-dimensional alkene modified antivirus photothermal nanofiber of the invention are further illustrated by the following specific examples.
Example 1
SnCl 2 ·2H 2 O and thioacetamide in a ratio of 1:1, respectively dispersing the mixture evenly in isopropanol, and magnetically stirring for 20min; then SnCl 2 ·2H 2 Evenly mixing the O and the thioacetamide dispersion liquid, and magnetically stirring for 30min; transferring the mixed solution into the inner liner of a polytetrafluoroethylene reaction kettle, and carrying out solvothermal reaction for 12h at 160 ℃; and after the reaction kettle is naturally cooled to room temperature, respectively centrifugally washing the reaction kettle for three times by using distilled water and absolute ethyl alcohol, and drying the reaction kettle in vacuum at 40 ℃ to obtain the SnS nanosheet.
And dispersing the SnS nanosheets in isopropanol with the concentration of 1.0mg/mL, and spraying the SnS nanosheets on the surface of the polypropylene melt-blown fabric by using a pressure spray gun to obtain the photo-thermal polypropylene melt-blown fabric loaded with the SnS nanosheets.
The new coronavirus resistant capability of the photo-thermal polypropylene melt-blown fabric loaded with the SnS nanosheets prepared in the embodiment is compared with that of the polypropylene melt-blown fabric which is not loaded with the SnS nanosheets in the attached figure 1.
Example 2
Mixing Ti 3 AlC 2 Slowly adding into hydrofluoric acid solution with concentration of 0.1g mL -1 Magnetically stirring at 30 deg.c for reaction for 12 hr; centrifuging the reacted solution at 3500rpm for 20min; then collecting the centrifuged precipitate, re-dispersing the precipitate in deionized water, filtering, and vacuum-drying to obtain etched multilayer Ti 3 C 2 T x A powder; taking the multilayer Ti obtained in the step 3 C 2 T x Powder prepared to a concentration of 2mg mL -1 Centrifuging the aqueous solution of (1) at 8000rpm for 30min; centrifuging the supernatant at 18000rpm for 30min, collecting the precipitate, and vacuum drying at 40 deg.C overnight to obtain Ti with small layer 3 C 2 T x A nanosheet.
Mixing Ti 3 C 2 T x Dispersing the nano-sheets in isopropanol at a concentration of 1.0mg/mL, and spraying Ti with a pressure spray gun 3 C 2 T x Spraying the nano sheet on the surface of polypropylene melt-blown cloth to obtain the loaded Ti 3 C 2 T x The photo-thermal polypropylene melt-blown fabric of the nano-sheets.
Example 3
Mixing Ti 3 AlC 2 Slowly adding the mixture into hydrofluoric acid solution with the concentration of 0.1g mL -1 Magnetically stirring at 30 deg.c for 12 hr; centrifuging the reacted solution at 3500rpm for 20min; then collecting the centrifuged precipitate, re-dispersing the precipitate in deionized water, filtering, and vacuum-drying to obtain etched multilayer Ti 3 C 2 T x Powder; taking the multilayer Ti obtained in the step 3 C 2 T x Powder, prepared to a concentration of 2mg mL -1 Centrifuging the aqueous solution of (1) at 8000rpm for 30min; centrifuging the supernatant at 18000rpm for 30min, collecting the precipitate, and vacuum drying at 40 deg.C overnight to obtain Ti with small layer 3 C 2 T x Nanosheets.
Mixing Ti 3 C 2 T x Dispersing the nano-sheets in isopropanol at the concentration of 1.0mg/mL, and completely soaking the polyester fiber melt-blown cloth in Ti 3 C 2 T x Isopropanol solution of the nanosheets; taking out the Ti after 20min and drying to obtain the loaded Ti 3 C 2 T x The photo-thermal polyester fiber of the nano-sheet is melt-blown.
Example 4
SnCl 2 ·2H 2 O and thioacetamide in a ratio of 1:1, respectively dispersing the mixture evenly in isopropanol, and magnetically stirring for 20min; then SnCl 2 ·2H 2 Evenly mixing the O and the thioacetamide dispersion liquid, and magnetically stirring for 30min; transferring the mixed solution into the inner liner of a polytetrafluoroethylene reaction kettle, and carrying out solvothermal reaction for 12h at 160 ℃; and after the reaction kettle is naturally cooled to room temperature, respectively centrifugally washing the reaction kettle for three times by using distilled water and absolute ethyl alcohol, and drying the reaction kettle in vacuum at 40 ℃ to obtain the SnS nanosheet.
And (2) dispersing the SnS nanosheets in isopropanol with the concentration of 1.5mg/mL, and spraying the SnS nanosheets on the surface of the polycarbonate electrospun cloth by using a pressure spray gun to obtain the photo-thermal polycarbonate electrospun cloth loaded with the SnS nanosheets.
Example 5
SnCl 2 ·2H 2 O and thioacetamide in a ratio of 1:1, respectively dispersing the mixture evenly in isopropanol, and magnetically stirring for 20min; then SnCl 2 ·2H 2 Uniformly mixing the O and the thioacetamide dispersion liquid, and magnetically stirring for 30min; transferring the mixed solution into a polytetrafluoroethylene reaction kettle lining, and carrying out solvothermal reaction for 12 hours at 160 ℃; and after the reaction kettle is naturally cooled to room temperature, respectively centrifugally washing the reaction kettle for three times by using distilled water and absolute ethyl alcohol, and drying the reaction kettle in vacuum at 40 ℃ to obtain the SnS nanosheet.
The SnS nanosheet is doped in the polypropylene electrospinning solution, the mass fraction of the SnS nanosheet is 5wt%, and the photo-thermal polypropylene electrospinning fabric loaded with the SnS nanosheet is prepared by a wet spinning technology.
Claims (8)
1. A preparation method of two-dimensional alkene modified antiviral photo-thermal nano-fiber is characterized by comprising the following steps: preparing a layered two-dimensional alkene nano sheet; and loading the layered two-dimensional alkene nano-sheet on the non-woven nano-fiber to obtain the non-woven antiviral fabric.
2. The method for preparing the antiviral photo-thermal nanofiber as claimed in claim 1, wherein the two-dimensional alkene modification method comprises the following steps: the two-dimensional alkene comprises one or two or three of graphene, MXene, silylene, germanium alkene, stannene, tellurium alkene, boron alkene materials and derivatives thereof.
3. The method for preparing the two-dimensional alkene modified antiviral photothermal nanofiber as claimed in claim 2, wherein: the synthetic method of the two-dimensional alkene nano-sheet is an inorganic acid etching method or a solvothermal method.
4. The method for preparing the two-dimensional alkene modified antiviral photothermal nanofiber as claimed in claim 1, wherein: the nano-fiber comprises one or two or three of polymers such as polypropylene, polyethylene, polyester fiber, polylactic acid, levorotatory polylactic acid, dextrorotatory polylactic acid, cellulose acetate, regenerated cellulose, polycarbonate, polyacrylonitrile, nylon fiber, polycaprolactone, polyethylene oxide, polyethylene glycol terephthalate, polyamide, polyimide, polystyrene, polyurethane, polyvinyl alcohol, polyvinylidene fluoride, collagen, chitosan, fibroin and the like.
5. The method for preparing the two-dimensional alkene modified antiviral photothermal nanofiber as claimed in claim 1, wherein: the preparation method of the two-dimensional alkene-loaded nanofiber comprises in-situ treatment and post-treatment, wherein the in-situ treatment is to mix precursor solutions of the two-dimensional alkene and the nanofiber and prepare the two-dimensional alkene-loaded nanofiber through a non-woven technology; and the post-treatment is to load the two-dimensional olefin nano-sheets on the non-woven nano-fibers by spraying, dip coating, spin coating, dipping-pulling or brush coating.
6. The method for preparing the antiviral photo-thermal nanofiber recited in claim 5, wherein the two-dimensional alkene modification method comprises the following steps: the non-weaving technology is one or two of spun-bonded non-weaving technology, melt-blown non-weaving technology, spun-bonded melt-blown composite non-weaving technology, wet non-weaving technology, spunlace non-weaving technology, needle non-manufacturing technology, thermal bonding non-weaving technology and pulp air-laid non-weaving technology.
7. The method for preparing the antiviral photo-thermal nanofiber as claimed in claim 1, wherein the two-dimensional alkene modification method comprises the following steps: the mass ratio of the layered two-dimensional olefin nano-sheets to the non-woven nano-fibers is 0-0.5.
8. The use of the antiviral photothermal nanofibers prepared by the preparation method as claimed in any one of claims 1 to 7 for the antiviral activity of neocoronaviruses.
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