CN113797649B - Antibacterial and antivirus air filtering material and preparation method thereof - Google Patents
Antibacterial and antivirus air filtering material and preparation method thereofDownload PDFInfo
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Abstract
Translated fromChinese
Description
Technical Field
The invention relates to the field of air purification materials, in particular to an antibacterial and antivirus air filter material and a preparation method thereof.
Background
The existing respiratory protection articles have the defects of larger straight fiber diameter, large aperture between fibers and poor protection and antibacterial effects, the research on the air filtering material capable of efficiently intercepting viruses and killing bacteria has great significance for the self protection of people, and the nanofiber air filtering material is expected to be further developed into a novel antibacterial and antivirus air filtering material by using the lower air resistance and the better PM2.5 interception effect.
The air filtering material with the two-dimensional net structure, which is formed by mutually overlapping common one-dimensional nanofibers (>200nm) and superfine nanofibers (<20nm), has the advantages of small fiber diameter, large specific surface area, small pore diameter, high porosity and the like, can effectively prevent the invasion of harmful particles, and simultaneously keeps higher air permeability, but the traditional manufacturing method is difficult to prepare the air filtering material and has poor process reproducibility. Meanwhile, the air filtering material has the functions of efficiently intercepting ultrafine virus particles and killing bacteria, and the problem that needs to overcome the excellent air permeability is solved.
Chinese patent publication No. CN101564914B discloses a method for preparing a nano-cobweb/nano-fiber composite protective material, which comprises preparing a spinning solution, and performing electrostatic spinning to obtain a protective material with a nano-cobweb composite nano-fiber structure. Wherein the average diameter of the nanometer spider web is about 15nm, the pore diameter is 10-80nm, and the nanometer spider web can effectively protect viruses with the diameters of 80-120nm, such as H1N1 influenza A, avian influenza, equine influenza, SARS pathogens, and the like. However, the preparation of the protective material needs to be completed by depending on a specific superfine nano spider web/nano fiber electrostatic spinning manufacturing device, and the requirements on spinning equipment and parameters are high.
Chinese patent publication No. CN108004682B discloses a method for preparing a positively charged hybrid fiber membrane by electrostatic spinning, which comprises the following steps: preparing ceramic precursor sol-gel, and preparing inorganic positively charged ceramic particles after vacuum freeze drying and calcining; then adding the inorganic positively charged ceramic particles into the polymer solution to obtain a spinning solution; preparing organic-inorganic hybrid fibers by electrostatic spinning; and finally, carrying out modification treatment on the organic-inorganic hybrid fiber to obtain the positively charged hybrid fiber membrane. The positively charged hybrid fiber membrane has good thermal stability, large specific surface area and excellent positively charged performance, and is expected to be applied to virus adsorption, but corresponding data do not exist in the invention to directly show that the positively charged hybrid fiber membrane has excellent virus adsorption and blocking performance.
Chinese patent publication No. CN113026428A discloses electrospun nano air filter paper for an air filter and a method for preparing the same, wherein the electrospun nano air filter paper is formed by compounding a polyvinyl alcohol layer and air filter paper; the polyvinyl alcohol layer is prepared by depositing polyvinyl alcohol solution on the air filter paper through electrostatic spinning. The electrostatic spinning nano air filter paper has the filtering efficiency of more than or equal to 99.95 percent for the particles with the diameter of more than or equal to 0.5 mu m, but does not have the capacities of resisting bacteria and blocking viruses.
Disclosure of Invention
The invention provides an antibacterial and antivirus air filter material which is simple in preparation method and convenient for large-scale production, has good air permeability, can keep excellent antibacterial and antivirus performance under lower air resistance, and can enhance the killing of bacteria and viruses by means of natural light.
The technical scheme is as follows:
a preparation method of an antibacterial and antivirus air filter material comprises the following steps:
(1) dissolving a high polymer material with strong dipole property in an organic solvent A, adding nano titanium dioxide, and uniformly dispersing to obtain a spinning solution;
(2) soaking the superfine nanofiber in a dopamine buffer solution to obtain dopamine-modified superfine nanofiber, performing antibacterial modification on the dopamine-modified superfine nanofiber to obtain antibacterial superfine nanofiber, and dispersing the antibacterial superfine nanofiber in an organic solvent B to obtain a spraying solution;
(3) spinning the spinning solution onto a collector through an electrostatic spinning technology to obtain a nanofiber supporting framework, and spraying the spraying solution onto the nanofiber supporting framework to obtain the antibacterial and anti-virus air filtering material.
The invention relates to an air filtering material with antibacterial and antivirus functions, which is characterized in that a physical and chemical structure of a nanofiber air filtering material is a main factor influencing the antibacterial and antivirus performance of the air filtering material.
The dipole-dipole effect is one of the main effects of intercepting viral bacteria. Therefore, the polymer material with large dipole moment has better effect of removing virus, bacteria and particles.
Preferably, the polymer material with strong dipole property comprises at least one of Polyacrylonitrile (PAN), polyvinylpyrrolidone (PVP) and polyvinyl alcohol (PVA), the dipole moment is 1.2-3.6D, the mass concentration is 10-30 wt%, and the weight-average molecular weight is 50,000-350,000.
Preferably, the organic solvent A comprises at least one of N-methylpyrrolidone, N-dimethylformamide and acetone.
Preferably, the nano titanium dioxide is anatase type nano titanium dioxide with the functions of photocatalytic oxidation and virus and bacteria killing; the mass concentration is 1-5 wt%.
The invention uses the superfine nano fiber to construct a fine filter network with good air permeability so as to realize the high-efficiency interception of virus and bacteria and the effective killing of the bacteria. The length-diameter ratio of the superfine nano-fiber is an important parameter, and the superfine nano-fiber with higher length-diameter ratio is easy to attach to the nano-fiber supporting framework and is not easy to fall off along with the flow of air.
The length-diameter ratio of the nanofiber refers to the ratio of the length to the diameter of the nanofiber, preferably, the diameter of the superfine nanofiber is 10-50 nm, and the length-diameter ratio is 100-1000; comprises at least one of cellulose nano-fiber, bacterial cellulose nano-fiber, copper nanowire, silver nanowire and silicon carbide nanowire.
Dopamine is a self-polymerization-adhesion material, can effectively modify the surface of the material, and the amino and quinoid structures of the dopamine can provide rich active sites for the functional modification of superfine nanofibers.
The preparation method of the dopamine buffer solution comprises the following steps: preparing a Tris-HCl buffer solution, adjusting the pH value to 7.5-9, and adding dopamine into the Tris-HCl buffer solution to obtain a dopamine buffer solution; preferably, the mass concentration of the dopamine in the dopamine buffer solution is 1-6 wt%.
Preferably, the soaking time of the superfine nano-fiber in the dopamine buffer solution is 0.1-10h, so as to avoid excessive self-aggregation of dopamine to influence the modification of the superfine nano-fiber surface.
Polylysine has rich amino groups, carboxyl groups, amido bonds and other groups, can be effectively combined with fine particles, and can generate electrophilic action with bacteria and penetrate through the outer wall of the bacteria to inhibit the synthesis of bacterial enzyme and protein, so that the aim of inhibiting the growth of the bacteria is fulfilled, and similarly, silver also has good bactericidal performance.
Preferably, the antibacterial modification method comprises the following steps: the method comprises the steps of soaking the dopamine-modified superfine nanofiber in a polylysine solution, obtaining the polylysine-modified antibacterial superfine nanofiber through Schiff base/Michael addition reaction between dopamine and polylysine, or soaking the dopamine-modified superfine nanofiber in a silver nitrate solution, and then dropwise adding ammonia water to obtain the silver-modified antibacterial superfine nanofiber.
Further preferably, the mass concentration of the polylysine solution is 1-10 wt%, and the pH value is 7.5-9; the mass concentration of the silver nitrate solution is 1-5 wt%, and the mass concentration of the ammonia water is 0.1-1 wt%; the soaking time of the dopamine modified superfine nano-fiber in polylysine or silver nitrate solution is 0.5-12 h.
The ultrafine nanofibers are easily entangled with each other and generate precipitates after being placed for a long time. Therefore, this phenomenon is prevented by controlling the concentration of the nanofibers, preferably, the concentration of the antibacterial ultrafine nanofibers in the spray coating liquid is 0.01 to 3 wt%.
Preferably, the organic solvent B includes at least one of acetone, ethanol, and isopropanol.
In the step (3), preferably, the electrostatic spinning parameters are as follows: the direct current voltage is 10-30kV, the flow rate of the spinning solution is 1-20mL/h, the ambient temperature is 20-30 ℃, the humidity is 20-40%, and the rotating speed of the collector is 0.1-1 m/min.
Preferably, the spraying process is as follows: spraying the spraying liquid onto the nanometer fiber support skeleton with a spray gun at a speed of 1-10mL/h, and accelerating solvent volatilization with infrared illumination.
The invention also discloses the antibacterial and antivirus air filter material prepared by the preparation method of the antibacterial and antivirus air filter material.
The antibacterial and antivirus air filter material has a fine filter network structure of a large-pore nano fiber support framework combined with a small pore, and the nano fiber support framework not only plays a supporting role, but also has the functions of photocatalysis killing, virus and bacteria interception and large particle interception; the fine filtering network has a small pore structure, and can intercept and kill viruses and bacteria.
Because the anatase type nano titanium dioxide has the function of killing viruses and bacteria by photocatalytic oxidation, the air filter material for resisting bacteria and viruses can enhance the killing of the viruses and bacteria by depending on natural light.
Preferably, the antibacterial and antivirus air filter material has a pressure drop of 14-21Pa, a sterilization rate of more than 99.5%, an interception rate of aerosol particles with a size of 100nm of more than 99.9%, and an average diameter of part of viruses of 100nm, so that the antibacterial and antivirus air filter material can keep excellent antibacterial and antivirus performance under low air resistance.
Compared with the prior art, the invention has the advantages that:
(1) the construction of the antibacterial and antivirus air filter material is realized by adopting a layer-by-layer stacking mode, a large-pore nano fiber supporting framework is constructed by utilizing an electrostatic spinning technology, and then superfine nano fibers are sprayed to construct a fine filter network with a small pore, so that virus and bacteria and the like can be efficiently intercepted; in addition, the superfine nano fiber has a certain sterilization function after being subjected to antibacterial modification, and the nano fiber supporting framework can also intercept virus and bacteria and the like through dipole-dipole effect.
(2) The introduction of the anatase type nano titanium dioxide with the function of killing virus and bacteria by photocatalytic oxidation also increases the killing effect of the air filter material for resisting bacteria and viruses under natural light.
(3) The antibacterial and antivirus air filter material disclosed by the invention is simple in preparation method, high in raw material utilization rate and convenient for large-scale production.
Drawings
FIG. 1 shows PAN-TiO in example 12SEM image of nanofiber support scaffold.
FIG. 2 is an SEM photograph of the antibacterial and antivirus air filtration material of example 1, with a scale of 3 μm.
FIG. 3 is an SEM partial enlarged view of the antibacterial and antivirus air filtration material of example 1, with a scale of 1 μm.
Detailed Description
The present invention is further illustrated by the following specific examples, but the scope of the present invention is not limited to the above-described examples.
Example 1
Dissolving PAN (with the weight-average molecular weight of 150,000 and the dipole moment of 3.6D) in N-methyl pyrrolidone, adding anatase type nano titanium dioxide, and uniformly dispersing to obtain a spinning solution, wherein the mass concentration of the PAN is 22 wt%, and the mass concentration of the anatase type nano titanium dioxide is 1 wt%; the anatase type nano titanium dioxide has the function of killing viruses and bacteria by photocatalytic oxidation.
Soaking a copper nanowire (with the diameter of 50nm and the length-diameter ratio of 800) in a dopamine buffer solution with the pH value of 8.5 and the mass concentration of 2 wt% for 30min, filtering to obtain a dopamine-modified copper nanowire, soaking the dopamine-modified copper nanowire in a polylysine solution with the pH value of 8.5 and the mass concentration of 2 wt% for 2h, collecting to obtain a polylysine-modified antibacterial nanofiber, and dispersing the antibacterial nanofiber in ethanol at the mass concentration of 3 wt% to obtain a spraying solution;
controlling the ambient temperature to be 30 ℃, the humidity to be 25-30%, the direct current voltage to be 10-13 kV, the spinning speed to be 5mL/h, and spinning the spinning solution on a rotary drum collector by utilizing the electrostatic spinning technology to obtain PAN-TiO2The nanofiber supports the skeleton, and at the same time, the spraying liquid is sprayed to PAN-TiO by a spray gun at the speed of 4mL/h2Supporting the skeleton with nanometer fiber and evaporating with infrared auxiliary solvent; and (4) performing electrostatic spinning and spraying for 2 hours to obtain the antibacterial and antivirus air filter material.
The antibacterial and antivirus air filter material has PAN-TiO2Fine filtering of copper nanowire modified by composite polylysine of nanofiber supporting frameworkThe network layer is stacked layer by layer.
PAN-TiO2SEM image of the nanofiber support scaffold is shown in fig. 1; an SEM image of the antibacterial and antivirus air filter material is shown in FIG. 2, and a partially enlarged view is shown in FIG. 3, wherein PAN-TiO2The diameter of the nano fiber is about 200nm, and the diameter of the polylysine modified copper nanowire is 50 nm.
Example 2
The high molecular material with strong dipole property is changed into PVP (weight average molecular weight is 50,000, dipole moment is 2.3D), the organic solvent of the spinning solution is changed into a 1:1 mixed solution of N, N-dimethylformamide and acetone, and other parameters and methods are the same as those of the example 1, so that the antibacterial and antivirus air filter material is obtained.
The antibacterial and antivirus air filter material has PVP-TiO2The structure that the nanofiber supporting framework is combined with the polylysine modified copper nanowire fine filtering network layer by layer is formed.
Example 3
The superfine nanofibers are replaced by cellulose nanofibers (diameter is 10nm, length-diameter ratio is 300), and other parameters and methods are the same as those in example 1, so that the antibacterial and antivirus air filter material is obtained.
The antibacterial and antivirus air filter material has PAN-TiO2The structure that the nanofiber supporting framework is combined with a polylysine modified cellulose nanofiber fine filtering network layer by layer is formed.
Example 4
The method comprises the steps of replacing the superfine nanofibers with cellulose nanofibers (the diameter is 10nm, the length-diameter ratio is 300), soaking the cellulose nanofibers in a dopamine buffer solution with the pH value of 8.5 and the mass concentration of 4 wt% for 20min, filtering to obtain dopamine-modified cellulose nanofibers, soaking the dopamine-modified cellulose nanofibers in a 2 wt% silver nitrate solution for 45min, then dropwise adding 0.5 wt% ammonia water, collecting the silver-modified antibacterial nanofibers, and obtaining the antibacterial and anti-virus air filter material with other parameters and methods the same as those in example 1.
The antibacterial and antivirus air filter material has PAN-TiO2Nanofiber support scaffoldThe composite silver-modified cellulose nanofiber fine filter network has a structure in which layers are stacked.
Example 5
The polymer material was changed to a mixture of PAN (weight average molecular weight of 150,000, dipole moment of 3.6D) and PVP (weight average molecular weight of 50,000, dipole moment of 2.3D) at a mass ratio of 1:1, the organic solvent of the dope was changed to a mixed solution of N, N-dimethylformamide and acetone (mass ratio of 2: 1), the sum of the mass concentrations of PAN and PVP in the dope was 25 wt%, and the other parameters and methods were the same as in example 4, to obtain an antibacterial and antivirus air filter material.
The antibacterial and antivirus air filter material has PAN-PVP-TiO2The structure that the nanofiber supporting framework is combined with the silver-modified cellulose nanofiber fine filtering network layer by layer is formed.
Example 6
The mass concentration of the polymer material in the spinning solution A is changed to 20 wt%, and the parameters of electrostatic spinning are as follows: the environment temperature is 30 ℃, the humidity is 25-30%, the direct current voltage is 20-25 kV, the spinning speed is 10mL/h, and other parameters and methods are the same as those in the example 1, so that the antibacterial and antivirus air filter material is obtained.
The antibacterial and antivirus air filter material has PAN-TiO2The structure that the nanofiber supporting framework is combined with the polylysine modified copper nanowire fine filtering network layer by layer is formed.
Sample analysis
The structure of the air filter material in the present invention was observed using a transmission electron microscope (SEM); the filtration performance of the air filtration material was calculated by the following formula, with the virus particles replaced by aerosol particles of comparable size:
the filtration performance is (1-air-permeable side aerosol concentration/air inlet side aerosol concentration) × 100%;
the antibacterial performance of the air filtration material was measured with a colony counter.
The SEM image shows that the antibacterial and antivirus air filter material has a structure that a nanofiber supporting framework is compounded with a fine filter network.
The performances of the antibacterial and antivirus air filter materials prepared in the embodiments 1 to 6 are shown in table 1, the antibacterial and antivirus air filter material prepared by the method has good air permeability, can achieve a sterilization rate of more than 99.5% while the pressure drop is 14-21Pa, has an interception rate of aerosol particles with the size of 100nm of more than 99.9%, and has an average diameter of part of viruses of about 100nm, so that the antibacterial and antivirus air filter material can keep excellent antibacterial and antivirus performances under low air resistance.
TABLE 1 Properties of antibacterial and antivirus air filtration materials prepared in examples 1 to 6
Claims (7)
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| CN114712937A (en)* | 2022-03-17 | 2022-07-08 | 固安县济科铁路机车配件有限公司 | Material, method and filter element for air filter element that can sterilize and virus in fresh air of air conditioner |
| CN114452729A (en)* | 2022-03-21 | 2022-05-10 | 南通康净环保科技有限公司 | Air filtering material with good virus filtering effect |
| CN115364692B (en)* | 2022-08-12 | 2023-08-25 | 中国科学院上海高等研究院 | A kind of air filtration composite membrane prepared based on cellulose nanofiber reinforced hydrogel conversion and its preparation method |
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- 2021-08-12CNCN202110924681.0Apatent/CN113797649B/enactiveActive
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