CN114917765A - Preparation method of antibacterial efficient low-resistance air filtering membrane made of fluff nanofibers - Google Patents

Preparation method of antibacterial efficient low-resistance air filtering membrane made of fluff nanofibers Download PDF

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CN114917765A
CN114917765A CN202210548584.0A CN202210548584A CN114917765A CN 114917765 A CN114917765 A CN 114917765A CN 202210548584 A CN202210548584 A CN 202210548584A CN 114917765 A CN114917765 A CN 114917765A
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efficiency low
antibacterial
resistance air
fluff
air filtration
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CN114917765B (en
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郑高峰
邵尊桂
肖钰洁
康国毅
陈华坛
姜佳昕
刘益芳
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Xiamen University
Shenzhen Research Institute of Xiamen University
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Shenzhen Research Institute of Xiamen University
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    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
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    • B01D67/0002—Organic membrane manufacture
    • A—HUMAN NECESSITIES
    • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N35/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having two bonds to hetero atoms with at the most one bond to halogen, e.g. aldehyde radical
    • A01N35/02—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having two bonds to hetero atoms with at the most one bond to halogen, e.g. aldehyde radical containing aliphatically bound aldehyde or keto groups, or thio analogues thereof; Derivatives thereof, e.g. acetals
    • A—HUMAN NECESSITIES
    • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
    • A01N43/02—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one or more oxygen or sulfur atoms as the only ring hetero atoms
    • A01N43/04—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one or more oxygen or sulfur atoms as the only ring hetero atoms with one hetero atom
    • A01N43/14—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one or more oxygen or sulfur atoms as the only ring hetero atoms with one hetero atom six-membered rings
    • A01N43/16—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one or more oxygen or sulfur atoms as the only ring hetero atoms with one hetero atom six-membered rings with oxygen as the ring hetero atom
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L9/00—Disinfection, sterilisation or deodorisation of air
    • A61L9/01—Deodorant compositions
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L9/00—Disinfection, sterilisation or deodorisation of air
    • A61L9/01—Deodorant compositions
    • A61L9/013—Deodorant compositions containing animal or plant extracts, or vegetable material
    • 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
    • B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
    • B01D69/08—Hollow fibre membranes
    • B01D69/081—Hollow fibre membranes characterised by the fibre diameter
    • 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
    • B01D69/08—Hollow fibre membranes
    • B01D69/085—Details relating to the spinneret
    • 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
    • B01D69/08—Hollow fibre membranes
    • B01D69/087—Details relating to the spinning process
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
    • B01D71/06—Organic material
    • B01D71/72—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, not provided for in a single one of the groups B01D71/46 - B01D71/70 and B01D71/701 - B01D71/702
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2257/00—Components to be removed
    • B01D2257/91—Bacteria; Microorganisms
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2258/00—Sources of waste gases
    • B01D2258/06—Polluted air
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2323/00—Details relating to membrane preparation
    • B01D2323/12—Specific ratios of components used
    • 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
    • B01D2325/02—Details relating to pores or porosity of the membranes
    • 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

Abstract

The invention relates to the field of air filtering materials, and discloses a preparation method of a down nanofiber antibacterial high-efficiency low-resistance air filtering membrane, which comprises the following steps: (1) dissolving polyoxyethylene, polycaprolactone, chitosan and curcumin in a solvent, and fully stirring to form a uniform and stable spinning solution; (2) the spinning solution obtained in the step (1) is used for electrostatic spinning to obtain the fluff nanofiber antibacterial high-efficiency low-resistance air filtration membrane with stable structure and performance, the air filtration membrane prepared by the method has high specific surface area, small pore diameter and ultrafine diameter, enhanced electrostatic effect can adsorb tiny particles, high-efficiency low-resistance high-performance air filtration is realized, meanwhile, antibacterial capability is enhanced due to successful introduction of a large amount of natural antibacterial agents and synergistic antibacterial effect of the natural antibacterial agents, nano toxicity is avoided, all components can be degraded, the high-efficiency low-resistance air filtration is realized, and meanwhile, the high-efficiency low-resistance air filtration membrane has strong antibacterial performance and degradability, and the application prospect is wide.

Description

Preparation method of antibacterial efficient low-resistance air filtering membrane made of fluff nano fibers
Technical Field
The invention relates to the field of air filtering materials, in particular to a preparation method of a down nanofiber antibacterial high-efficiency low-resistance air filtering membrane.
Background
Personal protection equipment is becoming more important, and the emphasis on realizing comfortable and safe personal protection lies in the development of high-efficiency low-resistance antibacterial air filtration membranes. The nanofiber prepared based on the electrostatic spinning technology is widely applied to realizing high-efficiency and low-resistance air filtration due to the advantages of small fiber diameter, large specific surface area, easiness in modification and the like. However, combining high efficiency, low resistance air filtration performance with safe, high efficiency antimicrobial performance presents a significant challenge. The prior art discloses a plurality of methods for preparing antibacterial nanofiber air filtration membranes, such as preparation and application of an antibacterial electrospinning nanofiber air filtration material (CN108993167A), an antibacterial composite nanofiber efficient air filtration material and a preparation method thereof (CN103520999A), a preparation method of an air filtration nanofiber membrane with a dendritic multi-stage structure (CN113430719A), a preparation method of an antibacterial nanofiber (CN113638073A) and the like, wherein the existing preparation methods are to endow the air filtration membrane with antibacterial performance by adding a natural antibacterial agent, but the prepared nanofiber filtration membranes cannot meet the requirements of high-efficiency and low-resistance air filtration. The patent CN113797649A discloses an antibacterial and antiviral air filtration material and a preparation method thereof, which realizes the development of an antibacterial high-efficiency low-resistance air filtration membrane by adding inorganic nanoparticles, however, the nano toxicity in the using process has potential safety hazard. In addition, the degradability of the air filter membrane is very important for environmental protection, and the influence of the waste filter material on the environment is reduced.
Disclosure of Invention
Therefore, a preparation method of the antibacterial efficient low-resistance air filtering membrane with the fluff nanofibers is needed to be provided, and the problem that the existing air filtering membrane cannot have degradability, strong antibacterial property, high efficiency and low resistance is solved.
In order to realize the aim, the invention provides a preparation method of a fluff nanofiber antibacterial high-efficiency low-resistance air filtration membrane, which comprises the following steps:
(1) dissolving polyoxyethylene, polycaprolactone, chitosan and curcumin in a solvent, and fully stirring to form a uniform and stable spinning solution;
(2) and (2) performing electrostatic spinning by using the spinning solution obtained in the step (1) to obtain the down nanofiber antibacterial high-efficiency low-resistance air filtering membrane with stable structure and performance.
Further, the mass fraction of the spinning solution is 10-20%.
Further, the mass fraction of the spinning solution is 12-14%.
Further, the mass ratio of the polyoxyethylene, the polycaprolactone, the chitosan and the curcumin in the spinning solution is 5-10:0.8-2:1-2: 0.3-1.
Further, the mass ratio of the polyethylene oxide, the polycaprolactone, the chitosan and the curcumin in the spinning solution is 7:1:1.5: 0.5.
Further, the solvent used in the step (1) is a mixed solution of formic acid and acetic acid, and the volume ratio of the formic acid to the acetic acid in the mixed solution is 1-3: 1-3.
Further, the electrostatic spinning conditions in the step (2) are as follows: the temperature is 10-50 ℃, the humidity is 30-60%, the spinning voltage is 20-26kV, the receiving distance is 10-20cm, and the liquid supply rate is 0.1-0.3 mL/h.
Further, in the step (1), the stirring time is 12-24 h.
The technical scheme has the following beneficial effects:
(1) in the preparation method provided by the invention, all the components are completely degradable polymers. By adding polycaprolactone, a polyethylene oxide and polycaprolactone system with low binding energy is constructed, in the system, the polycaprolactone only contains a large number of carbonyl groups as hydrogen bond acceptors, and a hydrogen bond donor is lacked, so that the binding energy of the system is reduced, and the voltage responsiveness is improved; in addition, chitosan containing a large amount of cations is further added into the blending system of the polyoxyethylene and the polycaprolactone, so that the conductivity of the solution is greatly improved; the addition of curcumin increases the variability of the composition of the solution, further promoting jet splitting. Finally, the jet flow realizes multi-stage splitting in the electrospinning process due to low combination energy, high conductivity and large component difference, a large number of superfine nanofiber structures are prepared, and the coverage rate is as high as 100%.
(2) The prepared antibacterial efficient low-resistance air filtering membrane with the fluff nano-fibers has the advantages that the antibacterial efficient low-resistance air filtering membrane has higher specific surface area, smaller pore size and enhanced electrostatic effect caused by extremely fine diameter, ultrafine particles can be effectively intercepted and adsorbed, the air filtering performance is greatly improved, the filtering efficiency of the air filtering membrane on PM0.3 reaches more than 99%, the resistance pressure drop does not exceed 60Pa, and efficient low-resistance air filtering is successfully realized.
(3) Due to the high loading of chitosan and curcumin and the synergistic antibacterial effect, the antibacterial performance of the villus nano air filtering membrane is greatly improved. The chitosan contains a large number of cationic groups, and can adsorb negatively charged bacterial cell membranes to break and die; the curcumin contains a large number of antioxidant factors and functional groups, can destroy cell walls of bacteria to increase the sensitivity of the bacteria to chitosan, and can inhibit a colony response mechanism of the bacteria, avoid the formation of bacterial biofilms and greatly reduce the drug resistance of the bacteria. Therefore, the prepared down feather nanofiber air filtering membrane can realize high-efficiency antibacterial performance, and the antibacterial rate to escherichia coli and staphylococcus aureus is not lower than 99%.
(4) The preparation process of the fluff nano air filtering membrane adopts the all-polymer solution to carry out one-step electrostatic spinning, so that the preparation efficiency is improved, the nano toxicity caused by the introduction of inorganic nano particles is effectively avoided, the preparation of the high-efficiency low-resistance air filtering membrane with safe, high-efficiency and antibacterial properties is realized, and the application field of the prepared fluff nano air filtering membrane is further widened.
Drawings
FIG. 1 is a schematic diagram of a preparation process of a fluff nanofiber antibacterial high-efficiency low-resistance air filter membrane.
FIG. 2 is a flow chart of the preparation of the down nanofiber antibacterial high-efficiency low-resistance air filtration membrane.
FIG. 3 is a schematic diagram of the electrostatic spinning splitting behavior of the down nanofiber antibacterial high-efficiency low-resistance air filtering membrane.
FIG. 4 is a scanning electron microscope photograph of the antibacterial high-efficiency low-resistance air filtration membrane made of the fluff nanofibers.
FIG. 5 is a scanning electron microscope photograph of a multi-stage split structure of down fibers of the down nanofiber antibacterial high-efficiency low-resistance air filtration membrane.
FIG. 6 is a scanning electron micrograph of a nanofiber membrane prepared by a low binding energy electrospinning system.
Fig. 7 is a scanning electron micrograph of the nanofiber membrane prepared by the moderate binding energy electrospinning system.
FIG. 8 is a scanning electron micrograph of a nanofiber membrane prepared by a high binding energy electrospinning system.
Detailed Description
To explain technical contents, structural features, and objects and effects of the technical solutions in detail, the following detailed description is given with reference to the accompanying drawings in conjunction with the embodiments.
The invention provides a preparation method of a down nanofiber antibacterial high-efficiency low-resistance air filtering membrane, which comprises the following steps:
(1) dissolving polyoxyethylene, polycaprolactone, chitosan and curcumin in a solvent, and fully stirring to form a uniform and stable spinning solution;
(2) and (2) performing electrostatic spinning by using the spinning solution obtained in the step (1) to obtain the antibacterial high-efficiency low-resistance air filtration membrane of the fluff nanofiber with stable structure and performance.
The flow of the preparation process is shown in fig. 1-2, in the electrospinning process of the spinning solution, splitting action occurs in electrospinning (as shown in fig. 3), the obtained air filtering membrane is a fluff nanofiber layer with multi-stage splitting, the average diameter of the fiber is 2-30nm, and the coverage rate is 100%. The fluff nano fiber layer is a fiber membrane material formed by mutually compounding superfine fluff fibers and one-dimensional nano fibers. The superfine fluff fiber has a two-dimensional structure with multi-stage splitting, the average diameter of the fiber is 2-30nm, and the coverage rate is 100%.
The specific embodiment is as follows:
example 1
Preparing 1/1 volume ratio compound organic solvent from 3.99g formic acid and 3.34g acetic acid at room temperature; respectively weighing 0.7g of polyethylene oxide, 0.1g of polycaprolactone, 0.15g of chitosan and 0.05g of curcumin according to the mass concentration of 12 wt%, respectively adding the materials into a compound organic solvent, and continuously stirring the materials for 24 hours by using a magnetic stirrer until the materials are fully dissolved to obtain a polyethylene oxide, polycaprolactone, chitosan and curcumin blended spinning solution with the mass ratio of 7/1/1.5/0.5.
Electrostatic spinning is carried out under the conditions that the temperature is 24 ℃, the humidity is 50%, the spinning voltage is 24kV, the receiving distance is 15cm, and the liquid supply rate is 0.15mL/h, so that the down nanofiber antibacterial high-efficiency low-resistance air filtering membrane (shown in figure 4) with high-efficiency low-resistance air filtering performance, safety high-efficiency antibacterial performance and 100% down coverage rate can be obtained, and the two-dimensional structure (shown in figure 5) with multi-stage splitting is formed.
Example 2
Preparing a compound organic solvent with the volume ratio of 1/1 by taking 3.64g of formic acid and 3.05g of acetic acid at room temperature; respectively weighing 0.7g of polyethylene oxide, 0.1g of polycaprolactone, 0.15g of chitosan and 0.05g of curcumin according to the mass concentration of 13 wt%, respectively adding the materials into a compound organic solvent, and continuously stirring the materials for 24 hours by using a magnetic stirrer until the materials are fully dissolved to obtain a polyethylene oxide, polycaprolactone, chitosan and curcumin blended spinning solution with the mass ratio of 7/1/1.5/0.5.
Electrostatic spinning is carried out at the temperature of 24 ℃, the humidity of 50 percent, the spinning voltage of 24kV, the receiving distance of 15cm and the liquid supply rate of 0.15mL/h, so that the down nanofiber antibacterial high-efficiency low-resistance air filtering membrane with high-efficiency low-resistance air filtering performance, safety, high-efficiency and antibacterial performance and 100 percent down coverage rate can be obtained, and the two-dimensional structure with multi-stage splitting is formed.
Example 3
Preparing a compound organic solvent with the volume ratio of 1/1 by taking 3.34g of formic acid and 2.81g of acetic acid at room temperature; respectively weighing 0.7g of polyethylene oxide, 0.1g of polycaprolactone, 0.15g of chitosan and 0.05g of curcumin according to the mass concentration of 14 wt%, respectively adding the materials into a compound organic solvent, and continuously stirring the materials for 24 hours by using a magnetic stirrer until the materials are fully dissolved to obtain a polyethylene oxide, polycaprolactone, chitosan and curcumin blended spinning solution with the mass ratio of 7/1/1.5/0.5.
Electrostatic spinning is carried out under the conditions that the temperature is 24 ℃, the humidity is 50%, the spinning voltage is 24kV, the receiving distance is 15cm, and the liquid supply rate is 0.15mL/h, so that the down nanofiber antibacterial high-efficiency low-resistance air filtering membrane which has high-efficiency low-resistance air filtering performance, safety high-efficiency antibacterial performance and 100% down coverage rate and has a multistage split two-dimensional structure can be obtained.
Example 4
Preparing a compound organic solvent with the volume ratio of 2/3 by taking 3.25g of formic acid and 4.08g of acetic acid at room temperature; respectively weighing 0.7g of polyethylene oxide, 0.1g of polycaprolactone, 0.15g of chitosan and 0.05g of curcumin according to the mass concentration of 12 wt%, respectively adding the materials into a compound organic solvent, and continuously stirring the materials for 24 hours by using a magnetic stirrer until the materials are fully dissolved to obtain a polyethylene oxide, polycaprolactone, chitosan and curcumin blended spinning solution with the mass ratio of 7/1/1.5/0.5.
Electrostatic spinning is carried out at the temperature of 24 ℃, the humidity of 50 percent, the spinning voltage of 26kV, the receiving distance of 16cm and the liquid supply rate of 0.2mL/h, so that the down nanofiber antibacterial high-efficiency low-resistance air filtering membrane with high-efficiency low-resistance air filtering performance, safety, high-efficiency and antibacterial performance and 100 percent down coverage rate can be obtained, and the two-dimensional structure with multi-stage splitting is formed.
Example 5
4.71g of formic acid and 2.62g of acetic acid are taken at room temperature to prepare a compound organic solvent with the volume ratio of 3/2; 0.7g of polyethylene oxide, 0.1g of polycaprolactone, 0.15g of chitosan and 0.05g of curcumin are weighed respectively according to the mass concentration of 12 wt% and added into the compound organic solvent respectively, and a magnetic stirrer is used for continuously stirring for 24 hours until the materials are fully dissolved, so that the polyethylene oxide, polycaprolactone, chitosan and curcumin blended spinning solution with the mass ratio of 7/1/1.5/0.5 is obtained.
Electrostatic spinning is carried out at the temperature of 22 ℃, the humidity of 45%, the spinning voltage of 26kV, the receiving distance of 17cm and the liquid supply rate of 0.2mL/h, so that the down nanofiber antibacterial high-efficiency low-resistance air filtering membrane with high-efficiency low-resistance air filtering performance, safety, high-efficiency and antibacterial performance and 100% down coverage rate can be obtained, and the two-dimensional structure with multi-stage splitting is formed.
Example 6
4.71g of formic acid and 2.62g of acetic acid are taken at room temperature to prepare a compound organic solvent with the volume ratio of 3/2; 0.7g of polyethylene oxide, 0.1g of polycaprolactone, 0.15g of chitosan and 0.05g of curcumin are weighed respectively according to the mass concentration of 12 wt% and added into the compound organic solvent respectively, and a magnetic stirrer is used for continuously stirring for 24 hours until the materials are fully dissolved, so that the polyethylene oxide, polycaprolactone, chitosan and curcumin blended spinning solution with the mass ratio of 7/1/1.5/0.5 is obtained.
Electrostatic spinning is carried out at the temperature of 20 ℃, the humidity of 40 percent, the spinning voltage of 24kV, the receiving distance of 15cm and the liquid supply rate of 0.15mL/h, so that the down nanofiber antibacterial high-efficiency low-resistance air filtering membrane with high-efficiency low-resistance air filtering performance, safety, high-efficiency and antibacterial performance and 100 percent down coverage rate can be obtained, and the two-dimensional structure with multi-stage splitting is formed.
The air filtration membranes prepared in examples 1 to 6 were tested for air filtration performance using sodium chloride aerosol particles with a diameter of 300nm, and the filtration efficiency was over 99% and the resistance pressure drop was not more than 60 Pa. The air filter membranes prepared in examples 1 to 6 adopt escherichia coli and staphylococcus aureus to test antibacterial performance according to GB/T20944.3-2008, the antibacterial rates of the escherichia coli and the staphylococcus aureus are not lower than 99%, and specific test results are shown in Table 1.
Table 1 performance of the fluff nanofiber antimicrobial high efficiency low resistance air filtration membranes prepared in examples 1-6.
Figure BDA0003653383200000071
As can be seen from Table 1, the antibacterial air filtering membrane prepared by the method has high filtering efficiency, low air resistance and strong antibacterial performance, and has filtering efficiency of more than 99 percent on sodium chloride particles with the size of 300nm under the condition that the pressure drop is lower than 60 Pa; meanwhile, the sterilization rate of the bacillus coli and the staphylococcus aureus is not lower than 99 percent. In addition, the air filter membrane has no nano toxicity, and meets the safety requirement of personal protection; all are degradable components, and can be completely degraded in natural environment. Therefore, the antibacterial efficient low-resistance air filtering membrane with the fluff nanofibers can realize safe personal protection on the premise of meeting high-efficiency low-resistance air filtering, and simultaneously reduces the burden of the waste air filtering material on the environment.
Example 7
Compared to example 1, the difference is that, during preparation: the mass fraction of the spinning solution is 10%, the mass ratio of polyethylene oxide, polycaprolactone, chitosan and curcumin in the spinning solution is 5/2/1/1, and electrostatic spinning is carried out under the conditions that the temperature is 50 ℃, the humidity is 30%, the spinning voltage is 26kV, the receiving distance is 20cm, and the liquid supply rate is 0.1mL/h, so that the air filtering membrane can be obtained.
Example 8
Compared to example 1, the difference is that, during preparation: the mass fraction of the spinning solution is 18%, the mass ratio of polyethylene oxide, polycaprolactone, chitosan and curcumin in the spinning solution is 10/2/2/0.3, and electrostatic spinning is carried out under the conditions that the temperature is 24 ℃, the humidity is 50%, the spinning voltage is 24kV, the receiving distance is 15cm, and the liquid supply rate is 0.25mL/h, so that the air filtering membrane can be obtained.
Example 9
In contrast to example 1, the difference is that, at the time of preparation: the mass fraction of the spinning solution is 20%, the mass ratio of polyoxyethylene, polycaprolactone, chitosan and curcumin in the spinning solution is 8/0.8/1/1, and electrostatic spinning is carried out under the conditions of 10 ℃ of temperature, 60% of humidity, 20kV of spinning voltage, 10cm of receiving distance and 0.3mL/h of liquid supply rate, so that the air filtering membrane can be obtained.
Further, in order to prove the high voltage responsiveness brought by the low-binding-energy electrospinning system constructed by the air filter membrane prepared by the invention, the low-binding-energy electrospinning system, the medium-binding-energy electrospinning system and the high-binding-energy electrospinning system are constructed, wherein the low-binding-energy electrospinning system comprises polyethylene oxide, polycaprolactone, chitosan and curcumin, and the mass ratio of the components is 7/1/1.5/0.5; the components of the medium binding energy system are polyethylene oxide, polyamide 6, chitosan and curcumin, and the mass ratio is 7/1/1.5/0.5, because the polyamide 6 has a donor and an acceptor of a hydrogen bond, the binding energy is improved; the components of the high binding energy system are polyoxyethylene, chitosan and curcumin, and the mass ratio is 8/1.5/0.5, because the polyoxyethylene has two hydroxyl groups which are not only donors of hydrogen bonds but also acceptors of the hydrogen bonds, the binding energy is highest. In the same case, the low binding energy system has the highest voltage responsiveness, and a large number of very fine (diameter <20nm) nanofibers appear (see fig. 6); moderate binding energy has moderate voltage responsiveness, with a small number of fine nanofibers present (see fig. 7); the voltage responsiveness of the high binding energy system is weakest, the fiber diameter is greatly increased, and only few thin nano fibers are provided (see figure 8)
It is noted that, herein, relational terms such as first and second, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "include", "including" or any other variations thereof are intended to cover non-exclusive inclusion, so that a process, method, article, or terminal device including a series of elements includes not only those elements but also other elements not explicitly listed or inherent to such process, method, article, or terminal device. Without further limitation, an element defined by the phrases "comprising … …" or "comprising … …" does not exclude the presence of additional elements in a process, method, article, or terminal that comprises the element. Further, herein, "greater than," "less than," "more than," and the like are understood to exclude the present numbers; the terms "above", "below", "within" and the like are to be understood as including the number.
Although the embodiments have been described, once the basic inventive concept is obtained, other variations and modifications of these embodiments can be made by those skilled in the art, so that the above embodiments are only examples of the present invention, and not intended to limit the scope of the present invention, and all equivalent structures or equivalent processes using the contents of the present specification and drawings, or any other related technical fields, which are directly or indirectly applied thereto, are included in the scope of the present invention.

Claims (8)

1. A preparation method of a down nanofiber antibacterial high-efficiency low-resistance air filtering membrane is characterized by comprising the following steps:
(1) dissolving polyoxyethylene, polycaprolactone, chitosan and curcumin in a solvent, and fully stirring to form a uniform and stable spinning solution;
(2) and (2) performing electrostatic spinning by using the spinning solution obtained in the step (1) to obtain the down nanofiber antibacterial high-efficiency low-resistance air filtering membrane with stable structure and performance.
2. The method for preparing the antibacterial high-efficiency low-resistance air filtration membrane made of the fluff nanofibers according to claim 1, wherein the mass fraction of the spinning solution is 10-20%.
3. The method for preparing the antibacterial high-efficiency low-resistance air filtering membrane with the fluff nano fibers as claimed in claim 2, wherein the mass fraction of the spinning solution is 12-14%.
4. The preparation method of the fluff nanofiber antibacterial high-efficiency low-resistance air filtration membrane as claimed in claim 1, wherein the mass ratio of polyethylene oxide, polycaprolactone, chitosan and curcumin in the spinning solution is 5-10:0.8-2:1-2: 0.3-1.
5. The preparation method of the fluff nanofiber antibacterial high-efficiency low-resistance air filtration membrane as claimed in claim 4, wherein the mass ratio of polyethylene oxide, polycaprolactone, chitosan and curcumin in the spinning solution is 7:1:1.5: 0.5.
6. The method for preparing the antibacterial efficient low-resistance air filtration membrane with the fluff nanofibers as claimed in claim 1, wherein the solvent used in the step (1) is a mixed solution of formic acid and acetic acid, and the volume ratio of the formic acid to the acetic acid in the mixed solution is 1-3: 1-3.
7. The method for preparing the antibacterial high-efficiency low-resistance air filtration membrane made of the fluff nanofibers according to claim 1, wherein the conditions of electrostatic spinning in the step (2) are as follows: the temperature is 10-50 ℃, the humidity is 30-60%, the spinning voltage is 20-26kV, the receiving distance is 10-20cm, and the liquid supply rate is 0.1-0.3 mL/h.
8. The preparation method of the fluff nanofiber antibacterial high-efficiency low-resistance air filtration membrane as claimed in claim 1, wherein in the step (1), the stirring time is 12-24 h.
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