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CN108993167B - Preparation and application of an antibacterial electrospinning nanofiber air filter material - Google Patents

Preparation and application of an antibacterial electrospinning nanofiber air filter material Download PDF

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CN108993167B
CN108993167B CN201810913718.8A CN201810913718A CN108993167B CN 108993167 B CN108993167 B CN 108993167B CN 201810913718 A CN201810913718 A CN 201810913718A CN 108993167 B CN108993167 B CN 108993167B
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polyvinyl alcohol
preparation
antibacterial
spinning
aqueous solution
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CN108993167A (en
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马贵平
张璐
聂俊
吕金艳
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Beijing University of Chemical Technology
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Beijing University of Chemical Technology
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
    • B01D69/12—Composite membranes; Ultra-thin membranes
    • 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
    • A41D13/1107—Protective face masks, e.g. for surgical use, or for use in foul atmospheres characterised by their shape
    • A41D13/1153—Protective face masks, e.g. for surgical use, or for use in foul atmospheres characterised by their shape with a hood
    • 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D46/00—Filters or filtering processes specially modified for separating dispersed particles from gases or vapours
    • B01D46/54—Particle separators, e.g. dust precipitators, using ultra-fine filter sheets or diaphragms
    • B01D46/543—Particle separators, e.g. dust precipitators, using ultra-fine filter sheets or diaphragms using membranes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
    • B01D67/0002—Organic membrane manufacture
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
    • B01D67/0002—Organic membrane manufacture
    • B01D67/0006—Organic membrane manufacture by chemical reactions
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
    • B01D69/02—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor characterised by their properties
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
    • B01D69/12—Composite membranes; Ultra-thin membranes
    • B01D69/125—In situ manufacturing by polymerisation, polycondensation, cross-linking or chemical reaction
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2323/00—Details relating to membrane preparation
    • B01D2323/30—Cross-linking
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2323/00—Details relating to membrane preparation
    • B01D2323/39—Electrospinning
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2325/00—Details relating to properties of membranes
    • B01D2325/48—Antimicrobial properties

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  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Health & Medical Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Physical Education & Sports Medicine (AREA)
  • Textile Engineering (AREA)
  • Artificial Filaments (AREA)
  • Nonwoven Fabrics (AREA)
  • Spinning Methods And Devices For Manufacturing Artificial Fibers (AREA)

Abstract

本发明公开了复合抗菌静电纺丝纳米纤维膜的制备和应用，本发明用于口罩用抗菌空气过滤材料，该材料采用聚乙烯醇、壳聚糖和乙烯基胺‑共聚‑3‑烯丙基‑5,5‑二甲基海因为原料，制备方法是将聚乙烯醇和壳聚糖混合均匀纺丝作为最里层和最外层纳米纤维膜，起到辅助抗菌作用和机械支撑作用。中间层为聚乙烯醇和乙烯基胺‑共聚‑3‑烯丙基‑5,5‑二甲基海因混合纺丝，起到主要抗菌作用。对纺丝完成的三层纳米纤维膜置于戊二醛蒸汽中进行交联处理。本发明制备方法简单易行，条件可控，且具有优良的拦截效果和杀菌效果，在口罩用抗菌过滤材料领域有重要的价值和意义。

Figure 201810913718

The invention discloses the preparation and application of a composite antibacterial electrospinning nanofiber membrane. The invention is used for an antibacterial air filter material for masks, and the material adopts polyvinyl alcohol, chitosan and vinylamine-copolymer-3-allyl ‑5,5‑Dimethyl hydantoin raw material, the preparation method is that polyvinyl alcohol and chitosan are mixed and spun uniformly as the innermost and outermost nanofiber membranes, which play an auxiliary antibacterial effect and a mechanical support role. The middle layer is mixed spinning of polyvinyl alcohol and vinylamine-copolymer-3-allyl-5,5-dimethyl hydantoin, which plays the main antibacterial effect. The spun three-layer nanofiber membrane was placed in glutaraldehyde vapor for cross-linking treatment. The preparation method of the invention is simple and feasible, the conditions are controllable, and the invention has excellent interception effect and sterilization effect, and has important value and significance in the field of antibacterial filter materials for masks.

Figure 201810913718

Description

Preparation and application of antibacterial electrostatic spinning nanofiber air filtering material
Technical Field
The invention belongs to the field of biomedical materials, and particularly relates to preparation of a multilayer nanofiber air filtering material with an antibacterial function.
Background
Nowadays, economy develops rapidly, people's living standard improves day by day, but also brings serious environmental problem simultaneously. Air pollution is increasingly serious, and a large amount of dust particles and bacteria and viruses are carried in polluted atmosphere and spread along with air flow, so that great trouble is caused to the health of people.
The electrostatic spinning technology is that polymer solution is charged in a high-voltage electric field, the surface tension of the polymer solution is overcome through electrostatic attraction, and the polymer solution is sprayed and stretched to obtain the fiber with the nanometer diameter. The nanofiber obtained by electrostatic spinning has the characteristics of large surface area, low porosity, small diameter and the like, is a very good filtering material, has high filtering efficiency on fine particles and bacteria and viruses, and has huge application prospect in the field of medical materials.
The hydantoin derivative is a novel halamine bactericide which has the characteristics of easy regeneration, good stability, high efficiency and broad-spectrum antibiosis. The N-vinylformamide-copolymerization-3-allyl-5, 5-dimethylhydantoin is a hydantoin derivative containing active amino, has antibacterial performance after chlorination, can achieve a strong sterilization effect in a short time, and has a chlorination regeneration characteristic.
Chitosan is a natural high molecular compound, is cheap and easy to obtain, has good biodegradability and biocompatibility, is nontoxic, has antibacterial property, and is widely applied to the field of medical materials. However, the chitosan needs to be in contact with bacteria for a long time to kill the bacteria, so that the application range of the chitosan is limited, and the chitosan has poor spinnability and is usually blended and spun with other materials.
Polyvinyl alcohol (PVA) is a water-soluble polymer, has good biodegradability, biocompatibility and chemical stability, is nontoxic, and has good spinnability and film-forming property. Meanwhile, the solvent of the polyvinyl alcohol is water, so that the use of toxic solvents can be avoided, and the polyvinyl alcohol can be widely applied as a good biomedical material.
Disclosure of Invention
The invention aims to provide a preparation method of an antibacterial electrospun nanofiber filtering material under the condition that the antibacterial and filtering effects of the existing mask are poor. The composite nanofiber membrane prepared by the method has high filtering efficiency and antibacterial function on particles in air, and can be used as a leading filtering layer of an air filtering device such as a mask.
The technical scheme adopted by the invention is as follows:
(1) heating in a water bath at 80 ℃ to dissolve polyvinyl alcohol, preparing a polyvinyl alcohol aqueous solution with a certain concentration, preparing a chitosan acetic acid solution with a certain concentration, mixing and stirring chitosan and polyvinyl alcohol according to a certain proportion for 1h, adding the mixture into an injector, adopting an aluminum foil as a collecting matrix, and spinning under a proper condition to obtain the nanofiber membrane.
(2) Weighing a certain mass of copolymer sample, dissolving the copolymer sample in the polyvinyl alcohol aqueous solution prepared in the step (1), mixing and stirring for 2 hours at room temperature to obtain a transparent solution, and spinning under appropriate conditions by taking the nanofiber membrane obtained by spinning in the step (1) as a collecting matrix to obtain two layers of nanofiber membranes.
(3) And (3) spinning by taking the nanofiber membrane obtained in the step (2) as a collecting matrix to obtain a three-layer nanofiber membrane.
(4) And (3) placing the three-layer composite nanofiber membrane in a dryer, performing crosslinking treatment by using glutaraldehyde steam, then placing the membrane in a vacuum drying oven for drying, and then placing the membrane in a 0.10% sodium hypochlorite solution for chlorination treatment.
(5) The permeability and efficiency of interception of particles were tested using sodium chloride aerosol particles having a diameter of 300 to 500 nm. And testing the antibacterial property of the prepared composite electrostatic spinning nanofiber membrane by adopting escherichia coli and staphylococcus aureus.
Preferably, the mass concentration of the polyvinyl alcohol aqueous solution is 8-10%, and if the concentration is too low, the solution viscosity is too small, so that the electrostatic spinning machine sprays liquid drops, and the liquid drops cannot be electrosprayed into filaments. If the concentration is too high, the viscosity of the solution is too high, the solution is difficult to form a cone at the tip of the needle head, and the silk cannot be produced.
Preferably, the concentration of the chitosan acetic acid solution is 1% -3%, the concentration of acetic acid is 1%, chitosan is difficult to dissolve in water and dilute acetic acid, and the decomposition of chitosan can be caused due to the excessively high concentration of acetic acid. If the concentration of chitosan is too high, the viscosity is high, and the spinning is difficult, and the chitosan itself is difficult to spin.
Preferably, the mass concentration ratio of the polyvinyl alcohol aqueous solution to the chitosan acetic acid solution is 1:1,2: 1,3: 1. when the proportion of polyvinyl alcohol is small, the spinning is difficult, and the chitosan is difficult to spin. The mass ratio of the polyvinyl alcohol aqueous solution to the copolymer sample is 1:1,2: 1,3:1.
Preferably, the environment temperature of the electric spraying is 10-50 ℃, the output voltage of the high-voltage power supply is 15-30KV, the distance between the receiving device and the spinneret orifice is 5-15cm, and the flow rate is 0.3-0.5 mL/h.
Preferably, the microorganisms tested for antibacterial activity using sodium chloride aerosol particles having a diameter of 300-500nm are Escherichia coli and Staphylococcus aureus.
The application of the composite electrostatic spinning nanofiber membrane is used as an antibacterial air filtering material for a mask, and sodium chloride aerosol particles are used for testing air permeability and interception efficiency of the particles, and meanwhile, the pressure drop of the composite electrostatic spinning nanofiber membrane can also be tested. The filtering efficiency can reach 95-99%, the pressure drop is 25-300Pa, and the filtering efficiency is superior to the N90 and N95 masks on the market. And testing the antibacterial property of the prepared composite electrostatic spinning nanofiber membrane by adopting escherichia coli and staphylococcus aureus. The bacteriostasis rate can reach 100 percent within 30 min.
Compared with the prior literature reports, the three-layer electrostatic spinning nanofiber membrane used as the antibacterial filter material for the mask has the following advantages:
(1) the preparation method is simple and feasible, the conditions are controllable, and the cost is low.
(2) The middle layer of the antibacterial nanofiber membrane is a mixed spinning membrane of a macromolecular antibacterial agent and polyvinyl alcohol, and plays a leading antibacterial role. The innermost layer and the outermost layer are spinning films formed by mixing chitosan acetic acid solution and polyvinyl alcohol aqueous solution, have an auxiliary antibacterial effect, and have a mechanical supporting effect after cross-linking. Meanwhile, the diameters of the three layers of nanofiber membranes and the thickness of the membranes can be manually controlled, the composite membrane has an interception effect on ultrafine particles and bacteria in the air, and the intercepted bacteria can be killed by hydantoin copolymer samples and chitosan on the fiber membranes.
(3) The nanofiber membrane contains the macromolecular antibacterial agent, so that the separation of the antibacterial agent in the using process can be avoided, and the stability of the filter material is improved.
(4) The mask made of the antibacterial nanofiber filtering material has good air permeability and can effectively intercept sodium chloride aerosol particles.
Drawings
FIG. 1 is a diagram of a simple electrospinning apparatus according to the present invention;
FIG. 2 is a scanning electron microscope image of the composite spinning fiber membrane prepared by the invention;
FIG. 3 is a scanning electron microscope image of the composite spinning fiber membrane prepared by the invention after being soaked in water;
figure 4 is a TGA profile of a composite spun fibrous membrane made according to the present invention.
Detailed Description
Example 1
Preparing 8% polyvinyl alcohol aqueous solution and 1% chitosan acetic acid solution, stirring and mixing the solutions uniformly according to the mass fraction ratio of 1:1, adding the mixture into an injector, and spinning by using an electrostatic spinning machine under the conditions that the output voltage of a high-voltage power supply is 20KV, the distance between a needle head and a receiving device is 10cm, and the flow rate is 0.3mL/h to obtain a first layer of nano-fiber membrane.
And (3) dissolving a copolymer sample in 8% polyvinyl alcohol aqueous solution in a ratio of 1:1, and performing electrostatic spinning by taking the fiber membrane obtained in the step as a collecting matrix to obtain two layers of fiber membranes.
And the same as the preparation method of the spinning solution of the first layer of spinning membrane, the two layers of fiber membranes obtained in the steps are used as collecting matrixes, and the three layers of fiber membranes are obtained by spinning.
And (3) placing the three-layer nanofiber membrane obtained by spinning in the step into a dryer, and carrying out steam crosslinking by using 50% glutaraldehyde.
Example 2
Preparing 9% polyvinyl alcohol aqueous solution and 2% chitosan acetic acid solution, stirring and mixing the two solutions uniformly according to the mass fraction ratio of 2:1, adding the mixture into an injector, and spinning by using an electrostatic spinning machine under the conditions that the output voltage of a high-voltage power supply is 25KV, the distance between a needle head and a receiving device is 15cm, and the flow rate is 0.4mL/h to obtain a first layer of nano-fiber membrane.
And (3) dissolving a copolymer sample in 9% polyvinyl alcohol aqueous solution in a ratio of 2:1, and performing electrostatic spinning by taking the fiber membrane obtained in the step as a collecting matrix to obtain two layers of fiber membranes.
And the same as the preparation method of the spinning solution of the first layer of spinning membrane, the two layers of fiber membranes obtained in the step (1) are used as collecting matrixes, and three layers of fiber membranes are obtained by spinning.
And (3) placing the three-layer nanofiber membrane obtained by spinning in the step into a dryer, and carrying out steam crosslinking by using 50% glutaraldehyde.
Example 3
Preparing a 10% polyvinyl alcohol aqueous solution and a 3% chitosan acetic acid solution, and mixing the two solutions in percentage by mass as 3:1, adding the mixture into an injector after uniformly stirring and mixing, and spinning by using an electrostatic spinning machine under the conditions that the output voltage of a high-voltage power supply is 15KV, the distance between a needle head and a receiving device is 5cm, and the flow rate is 0.5mL/h to obtain a first layer of nanofiber membrane.
And (3) dissolving a copolymer sample in 10% polyvinyl alcohol aqueous solution in a ratio of 3:1, and performing electrostatic spinning by taking the fiber membrane obtained in the step as a collecting matrix to obtain two layers of fiber membranes.
And the same as the preparation method of the spinning solution of the first layer of spinning membrane, the two layers of fiber membranes obtained in the step (1) are used as collecting matrixes, and three layers of fiber membranes are obtained by spinning.
And (3) placing the three-layer nanofiber membrane obtained by spinning in the step into a dryer, and carrying out steam crosslinking by using 50% glutaraldehyde.
Example 4
Preparing a 10% polyvinyl alcohol aqueous solution and a 3% chitosan acetic acid solution, uniformly stirring and mixing the polyvinyl alcohol aqueous solution and the chitosan acetic acid solution according to the mass fraction ratio of 1:1, adding the mixture into an injector, and spinning by using an electrostatic spinning machine under the conditions that the output voltage of a high-voltage power supply is 15KV, the distance between a needle head and a receiving device is 10cm, and the flow rate is 0.3mL/h to obtain a first layer of nanofiber membrane.
And (3) dissolving a copolymer sample in 10% polyvinyl alcohol aqueous solution in a ratio of 1:1, and performing electrostatic spinning by taking the fiber membrane obtained in the step as a collecting matrix to obtain two layers of fiber membranes.
And the same as the preparation method of the spinning solution of the first layer of spinning membrane, the two layers of fiber membranes obtained in the step (1) are used as collecting matrixes, and three layers of fiber membranes are obtained by spinning.
And (3) placing the three-layer nanofiber membrane obtained by spinning in the step into a dryer, and carrying out steam crosslinking by using 50% glutaraldehyde.
Example 5
Preparing a 10% polyvinyl alcohol aqueous solution and a 3% chitosan acetic acid solution, uniformly stirring and mixing the solutions according to the mass ratio of 2:1, adding the solutions into an injector, and spinning by using an electrostatic spinning machine under the conditions that the output voltage of a high-voltage power supply is 20KV, the distance between a needle head and a receiving device is 15cm, and the flow rate is 0.4mL/h to obtain a first layer of nano-fiber membrane.
And (3) dissolving a copolymer sample in 10% polyvinyl alcohol aqueous solution in a ratio of 2:1, and performing electrostatic spinning by taking the fiber membrane obtained in the step as a collecting matrix to obtain two layers of fiber membranes.
And the same as the preparation method of the spinning solution of the first layer of spinning membrane, the two layers of fiber membranes obtained in the step (1) are used as collecting matrixes, and three layers of fiber membranes are obtained by spinning.
And (3) placing the three-layer nanofiber membrane obtained by spinning in the step into a dryer, and carrying out steam crosslinking by using 50% glutaraldehyde.
Example 6
Preparing a 10% polyvinyl alcohol aqueous solution and a 3% chitosan acetic acid solution, uniformly stirring and mixing the polyvinyl alcohol aqueous solution and the chitosan acetic acid solution according to the mass fraction ratio of 3:1, adding the mixture into an injector, and spinning by using an electrostatic spinning machine under the conditions that the output voltage of a high-voltage power supply is 25KV, the distance between a needle head and a receiving device is 15cm, and the flow rate is 0.5mL/h to obtain a first layer of nanofiber membrane.
And (3) dissolving the copolymer sample in 10% polyvinyl alcohol aqueous solution according to the mass fraction ratio of 3:1, and performing electrostatic spinning by taking the fiber membrane obtained in the step as a collecting matrix to obtain two layers of fiber membranes.
And the same as the preparation method of the spinning solution of the first layer of spinning membrane, the two layers of fiber membranes obtained in the step (1) are used as collecting matrixes, and three layers of fiber membranes are obtained by spinning.
And (3) placing the three-layer nanofiber membrane obtained by spinning in the step into a dryer, and carrying out steam crosslinking by using 50% glutaraldehyde.
Example 7
Preparing a 10% polyvinyl alcohol aqueous solution and a 3% chitosan acetic acid solution, and mixing the two solutions in percentage by mass as 3:1, adding the mixture into an injector after uniformly stirring and mixing, and spinning by using an electrostatic spinning machine under the conditions that the output voltage of a high-voltage power supply is 20KV, the distance between a needle head and a receiving device is 15cm, and the flow rate is 0.5mL/h to obtain a first layer of nanofiber membrane.
And (2) dissolving a copolymer sample in 10% polyvinyl alcohol aqueous solution according to the mass fraction ratio of 1:1, and performing electrostatic spinning by taking the fiber membrane obtained in the step as a collecting matrix to obtain a two-layer fiber membrane.
And the same as the preparation method of the spinning solution of the first layer of spinning membrane, the two layers of fiber membranes obtained in the step (1) are used as collecting matrixes, and three layers of fiber membranes are obtained by spinning.
And (3) placing the three-layer nanofiber membrane obtained by spinning in the step into a dryer, and carrying out steam crosslinking by using 50% glutaraldehyde.
In the above embodiment, the composite nanofiber membrane can be prepared by adjusting the ratio of the polymer in the spinning solution, the concentration of the polymer and the electrostatic spinning parameters according to experimental operations, so that the composite nanofiber membrane has the optimal filtration efficiency. It should be noted that the above embodiments are non-limiting examples of the present invention, and the present invention is not limited to the above embodiments, and many modifications can be made, and all modifications that can be derived from the present invention are considered to be within the scope of the present invention.

Claims (6)

1.抗菌的静电纺丝纳米纤维空气过滤材料的制备方法，其特征在于所述方法包括以下步骤：1. the preparation method of antibacterial electrospinning nanofiber air filter material is characterized in that described method comprises the following steps: (1)80℃水浴加热溶解聚乙烯醇，配制一定浓度的聚乙烯醇水溶液，同时配制一定浓度的壳聚糖乙酸溶液，将壳聚糖乙酸溶液和聚乙烯醇水溶液按照一定的比例进行混合搅拌1h，并将其加入注射器中，采用铝箔作为收集基体，在合适条件下纺丝得到纳米纤维膜；(1) Dissolve polyvinyl alcohol by heating in a water bath at 80°C, prepare a certain concentration of polyvinyl alcohol aqueous solution, and at the same time prepare a certain concentration of chitosan acetic acid solution, mix and stir the chitosan acetic acid solution and the polyvinyl alcohol aqueous solution according to a certain proportion 1h, add it into the syringe, use aluminum foil as the collection matrix, and spin under suitable conditions to obtain a nanofiber membrane; (2)称取一定质量的共聚物样品溶解于步骤(1)配置的聚乙烯醇水溶液，室温下混合搅拌2h，得到透明溶液，采用步骤(1)得到的纺在铝箔上的纳米纤维膜作为收集基体，在合适条件下纺丝得到两层纳米纤维膜；(2) Weigh a certain mass of copolymer sample and dissolve it in the polyvinyl alcohol aqueous solution prepared in step (1), mix and stir at room temperature for 2 hours to obtain a transparent solution, and use the nanofiber film spun on aluminum foil obtained in step (1) as the Collect the matrix and spin under suitable conditions to obtain two layers of nanofiber membrane; (3)采用步骤(2)得到的纳米纤维膜作为收集基体，进行纺丝，得到三层纳米纤维膜；(3) using the nanofiber membrane obtained in step (2) as a collection matrix, and spinning to obtain a three-layer nanofiber membrane; (4)将三层复合纳米纤维膜置于干燥器中，使用戊二醛蒸汽交联处理之后放于真空干燥箱烘干，然后置于0.10％次氯酸钠溶液中进行氯化处理；(4) placing the three-layer composite nanofiber membrane in a desiccator, using glutaraldehyde vapor cross-linking treatment, placing it in a vacuum drying oven for drying, and then placing it in a 0.10% sodium hypochlorite solution for chlorination; 所述共聚物样品为N-乙烯基甲酰胺-共聚-3-烯丙基-5,5-二甲基海因，是一种含活泼氨基海因衍生物共聚材料，其特征为结构式如下：The copolymer sample is N-vinylformamide-copolymerization-3-allyl-5,5-dimethyl hydantoin, which is a copolymer material containing active amino hydantoin derivatives, and is characterized by the following structural formula:
Figure FDA0002728035590000011
Figure FDA0002728035590000011
 2.根据权利要求1所述的制备方法，其特征在于：聚乙烯醇水溶液的质量分数为8％-10％，壳聚糖乙酸溶液质量分数为1％-3％。2 . The preparation method according to claim 1 , wherein the mass fraction of the polyvinyl alcohol aqueous solution is 8%-10%, and the mass fraction of the chitosan acetic acid solution is 1%-3%. 3 . 3.根据权利要求1所述的制备方法，其特征在于：纺丝环境温度为10-50℃，高压电源输出电压为15-30KV，接收装置与喷丝口之间的距离为5-15cm，流速为0.3-0.5mL/h。3. preparation method according to claim 1 is characterized in that: spinning environment temperature is 10-50 ℃, high-voltage power supply output voltage is 15-30KV, and the distance between receiving device and spinneret is 5-15cm, The flow rate was 0.3-0.5 mL/h. 4.根据权利要求1所述的制备方法，其特征在于：聚乙烯醇水溶液和壳聚糖乙酸溶液的质量比为1：1，2：1，3：1，聚乙烯醇水溶液和共聚物样品质量比为1：1，2：1，3:1。4. preparation method according to claim 1 is characterized in that: the mass ratio of polyvinyl alcohol aqueous solution and chitosan acetic acid solution is 1: 1, 2: 1, 3: 1, polyvinyl alcohol aqueous solution and copolymer sample The mass ratio is 1:1, 2:1, 3:1. 5.根据权利要求1所述的制备方法，其特征在于：作为口罩用抗菌过滤材料，使用具有300至500nm直径的氯化钠气溶胶颗粒测试透气性和对颗粒的拦截效率，其过滤效率可达95％-99％，压降为25-300Pa，优于市面上N90，N95口罩。5. preparation method according to claim 1 is characterized in that: as mask with antibacterial filter material, use the sodium chloride aerosol particle with 300 to 500nm diameter to test air permeability and the interception efficiency to particle, its filtration efficiency can be Up to 95%-99%, the pressure drop is 25-300Pa, which is better than N90 and N95 masks on the market. 6.根据权利要求1所述的制备方法，其特征在于：采用大肠杆菌和金黄色葡萄球菌测试制备的复合静电纺纳米纤维膜的抗菌性，在30min内可达到100％的抑菌率。6 . The preparation method according to claim 1 , wherein the antibacterial properties of the composite electrospinning nanofiber membrane prepared by using Escherichia coli and Staphylococcus aureus are tested, and the antibacterial rate of 100% can be achieved within 30 minutes. 7 .
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