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CN113457477A - Nanofiber filtering membrane and preparation method and application thereof - Google Patents

Nanofiber filtering membrane and preparation method and application thereof Download PDF

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Publication number
CN113457477A
CN113457477A CN202110929883.4A CN202110929883A CN113457477A CN 113457477 A CN113457477 A CN 113457477A CN 202110929883 A CN202110929883 A CN 202110929883A CN 113457477 A CN113457477 A CN 113457477A
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nanofiber
woven fabric
filtration membrane
electret
spinning
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Inventor
陈柔羲
王湘麟
陈明伊
陈健
朱自辉
曾元
张化
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Taizhou Shennan Navitas New Material Technology Co ltd
Taizhou Research Institute Of South University Of Science And Technology
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Taizhou Shennan Navitas New Material Technology Co ltd
Taizhou Research Institute Of South University Of Science And Technology
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Priority to CN202110929883.4A priority Critical patent/CN113457477A/en
Publication of CN113457477A publication Critical patent/CN113457477A/en
Priority to PCT/CN2021/142315 priority patent/WO2023015826A1/en
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    • 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
    • B01D71/30—Polyalkenyl halides
    • 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
    • B01D67/0079—Manufacture of membranes comprising organic and inorganic components
    • 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
    • B01D69/08—Hollow fibre membranes
    • 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
    • B01D71/38—Polyalkenylalcohols; Polyalkenylesters; Polyalkenylethers; Polyalkenylaldehydes; Polyalkenylketones; Polyalkenylacetals; Polyalkenylketals
    • 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
    • B01D71/40—Polymers of unsaturated acids or derivatives thereof, e.g. salts, amides, imides, nitriles, anhydrides, esters
    • B01D71/42—Polymers of nitriles, e.g. polyacrylonitrile
    • 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
    • B01D71/58—Other polymers having nitrogen in the main chain, with or without oxygen or carbon only
    • 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
    • B01D71/58—Other polymers having nitrogen in the main chain, with or without oxygen or carbon only
    • B01D71/62—Polycondensates having nitrogen-containing heterocyclic rings in the main chain
    • B01D71/64—Polyimides; Polyamide-imides; Polyester-imides; Polyamide acids or similar polyimide precursors
    • 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
    • B01D71/66—Polymers having sulfur in the main chain, with or without nitrogen, oxygen or carbon only
    • B01D71/68—Polysulfones; Polyethersulfones
    • 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 & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Inorganic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Filtering Materials (AREA)

Abstract

本发明涉及一种纳米纤维过滤膜及其制备方法和应用，所述纳米纤维过滤膜包括聚合物纤维以及附着在所述聚合物纤维表面的驻极纳米颗粒和ZnAc·2H2O。ZnAc·2H2O与驻极纳米颗粒协同作用，能够有效促进驻极纳米颗粒的驻极效果，使纳米纤维膜可以更加高效的捕捉直径较小的气溶胶，并且具有较低的滤阻，即具有高效低阻的性能，同时，还能够有效提高纳米纤维膜的抑菌性能，可以用于口罩、防护服等防护用品中。

Figure 202110929883

The invention relates to a nanofiber filter membrane, a preparation method and application thereof. The nanofiber filter membrane comprises polymer fibers, electret nanoparticles and ZnAc·2H 2 O attached to the surface of the polymer fibers. The synergistic effect of ZnAc·2H 2 O and electret nanoparticles can effectively promote the electret effect of electret nanoparticles, so that the nanofiber membrane can more efficiently capture aerosols with smaller diameters and has a lower filtration resistance, namely It has the properties of high efficiency and low resistance, and at the same time, it can also effectively improve the antibacterial properties of the nanofiber membrane, and can be used in protective equipment such as masks and protective clothing.

Figure 202110929883

Description

Nanofiber filtering membrane and preparation method and application thereof
Technical Field
The invention relates to the technical field of aerosol protection, in particular to a nanofiber filtering membrane and a preparation method and application thereof, and particularly relates to a nanofiber filtering membrane for efficiently capturing aerosol and a preparation method and application thereof.
Background
Aerosol refers to droplets having a diameter of less than 5 microns. Smaller, lighter aerosols can remain and accumulate in the air, and if they contain viruses, they can be transmitted over great distances by airflow, leading to disease. Therefore, research on effective interception of aerosols is particularly important.
At present, the nanofiber filtering membrane in the prior art has the characteristics of small wire diameter, high porosity, large specific surface area and the like, shows higher filtering efficiency compared with the conventional non-woven filtering membrane, and is widely used in the fields of air filtration, sewage filtration and the like. However, with the development of the times, the performance requirements on the filter material are higher and higher, and for effectively intercepting aerosol with smaller diameter, development of a filter membrane with lower resistance and higher efficiency is urgently needed.
CN106310782A discloses a nanofiber filtration membrane and a nanofiber composite filtration membrane, in which the nanofibers have a hollow structure with a through-hole on the surface layer, which can improve the filtration efficiency and reduce the air resistance, and have a longer service life. The nanofiber filtering membrane and the preparation method of the nanofiber composite filtering membrane are prepared through coaxial electrostatic spinning. The air filter has wide application value in the field of air filtration, and has great application prospect in products such as air purifiers, automobile filter elements, masks and the like. However, the nanofiber filter membrane cannot achieve the effect of efficiently trapping aerosol.
CN107455822A discloses a nanofiber-microfiber composite haze-preventing mask, which not only has the characteristics of low air resistance and high filtering efficiency for particulate pollutants, but also can filter volatile organic compounds, acidic gases, alkaline gases, nitrogen oxides, sulfur oxides, carbon monoxide, or eliminate smoke, odor, formaldehyde, and the like, and can be used for protection of various polluted gas scenes. The nanofiber-micron fiber composite haze-prevention mask comprises at least one micron fiber layer and is arranged on the inner side of the micron fiber layer, functional additives are added into the nanofibers of the nanometer fiber layer, and the functional additives comprise a VOC adsorbent, an acid adsorbent, an alkaline adsorbent, a bactericide, an antiviral agent, a photodegradation catalyst for decomposing VOC, a formaldehyde catalytic oxidant and a carbon monoxide adsorbent. The nano fiber-micron fiber composite haze-preventing mask has poor aerosol protection effect and cannot realize efficient capture of aerosol.
Therefore, there is a need in the art to develop a filter membrane that can efficiently capture aerosols and has a low filtration resistance.
Disclosure of Invention
In view of the disadvantages of the prior art, it is an object of the present invention to provide a nanofiber filtration membrane, and more particularly, to provide a nanofiber filtration membrane that efficiently traps aerosols. The nanofiber filtering membrane can efficiently block aerosol, has low filtration resistance and has excellent antibacterial performance.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention provides a nanofiber filter membrane for efficiently capturing aerosol, which comprises polymer fibers, and electret nanoparticles and ZnAc & 2H attached to the surfaces of the polymer fibers2O。
In the invention, the electret nanoparticles refer to electrolyte materials which can store space charges injected from the outside and polarization charges formed by freezing oriented dipoles for a long time and show electrostatic effect under certain conditions.
The invention introduces electret nano-particles and ZnAc & 2H on the surface of polymer fiber at the same time2And on one hand, the electret nanoparticles are adsorbed on the polymer fibers to form nanofiber filtering membrane fibers with charges carried on the surfaces, so that the electrostatic adsorption effect is achieved, aerosol particles in the air can be rapidly separated from the original streamline and adsorbed by the fibers, and the filtering efficiency of the aerosol with the smaller diameter is greatly improved. On the other hand, the addition of the electret nano-particles enables the surface of the fiber to have a large number of bulges, the specific surface area is increased, the filtration resistance is effectively reduced, and the fiber has an excellent self-cleaning function.
ZnAc·2H2The addition of O can effectively promote the electret effect of electret nano particles, so that the nanofiber membrane can more efficiently capture aerosol with smaller diameter, has lower filtration resistance, can effectively improve the antibacterial performance of the nanofiber membrane, and can be used for protective articles such as masks and protective clothing.
Preferably, the electret nanoparticles comprise silicon dioxide (SiO)2) Zif-8, tetraoxyethylene (PTFE), boehmite, barium titanate (BaTiO)3) Or silicon nitride (Si)3N4) Any one or a combination of at least two of them, preferably silica.
Using silicon dioxide (SiO)2) Nano particles such as Zif-8, PTFE and the like are added into a polymer spinning solution, an electret enhanced nano fiber film is prepared after electrostatic spinning, the filtration efficiency of a finally prepared filtration film on aerosol is greatly improved, the filtration film is particularly excellent in the interception performance of the aerosol with smaller diameter, and the addition of the particles enables the fibers to have good interception performance on the aerosol with smaller diameterThe surface of the filter membrane is provided with a large number of bulges, so that the specific surface area is increased, the filtration resistance is effectively reduced, and the purposes of improving the filtration efficiency of the filter membrane and reducing the filtration resistance are achieved.
Preferably, the particle size of the electret nanoparticles is 1000nm or less.
Preferably, the polymer fibers include any one or at least two combinations of polyvinyl chloride (PVDF) fibers, Polyacrylonitrile (PAN) fibers, Polyethersulfone (PES) fibers, Polyurethane (PU) fibers, polyvinyl alcohol (PVA) fibers, or polyvinyl pyrrolidone (PVP) fibers.
Preferably, the electret nanoparticles and ZnAc 2H2The mass ratio of O is 1 (0.2-10), for example, 1:0.5, 1:1, 1:2, 1:3, 1:4, 1:5, 1:6, 1:7, 1:8, 1:9, etc., preferably 1 (1-4).
The invention selects the electret nanometer particles and ZnAc.2H2And the O is compounded according to the mass ratio, so that the filtering efficiency can be further improved, the filtering resistance is reduced, the smooth spinning of the polymer fiber is ensured, if the addition amount of the electret nanoparticles is too much, a charge transfer channel can be formed, the charge storage capacity of the nanofiber membrane is reduced, the electret performance is reduced on the contrary, and meanwhile, along with the increase of the gram weight, the continuity of the spinning solution can be hindered to a certain extent, the entanglement of molecular chains is influenced, and the formation of coarse knots is caused. If ZnAc 2H2Too much addition of O can cause the spinning solution to be sticky, difficult to spin and reduce the uniformity of the fiber.
Preferably, the nanofiber filtration membrane has an efficiency > 93% for aerosol filtration, such as 93.2%, 95.18%, 99.155%, 99.8%, etc.
Preferably, the nanofiber filtration membrane has a gas resistance < 385Pa, such as 115Pa, 261.4Pa, 381.4Pa, etc.
Another object of the present invention is to provide a method for producing a nanofiber filtration membrane according to the first object, the method comprising: the electret nano-particles and ZnAc 2H are contained2And O and the spinning solution of the polymer are subjected to electrostatic spinning, and the nanofiber filtering membrane is obtained on a receiving substrate.
Preferably, in the spinning solution, ZnAc 2H2The mass ratio of O is 1% to 30%, for example, 2%, 3%, 4%, 5%, 6%, 7%, 8%, 9%, 10%, 11%, 12%, 13%, 14%, 15%, 16%, 17%, 18%, 19%, 20%, 21%, 22%, 23%, 24%, 25%, 26%, 27%, 28%, 29%, etc., preferably 5% to 20%.
Preferably, the mass ratio of the electret nanoparticles in the spinning solution is 3% to 8%, such as 4%, 5%, 6%, 7%, etc., preferably 5%.
Preferably, the receiving substrate includes any one of a polypropylene spunbonded nonwoven fabric, a polypropylene meltblown nonwoven fabric, a polyethylene terephthalate meltblown nonwoven fabric, a natural fiber woven fabric and knitted fabric, a chemical fiber woven fabric and knitted fabric, and a blended woven fabric and knitted fabric.
Preferably, the polymer comprises any one or a combination of at least two of polyvinyl chloride, polyacrylonitrile, polyethersulfone, polyurethane, polyvinyl alcohol, or polyvinylpyrrolidone. The corresponding molecular weight polymer can be selected and the concentration of the polymer can be adjusted according to the performance and the appearance of the required nanofiber membrane.
Preferably, the temperature of the electrospinning is 20 to 30 ℃, such as 21 ℃, 22 ℃, 23 ℃, 24 ℃, 25 ℃, 26 ℃, 27 ℃, 28 ℃, 29 ℃ and the like, preferably 25 ℃.
Preferably, the moisture of the electrospinning is 40% to 60%, such as 42%, 44%, 46%, 48%, 50%, 52%, 54%, 56%, 58%, etc., preferably 50%.
Preferably, the voltage of the electrospinning is 15-80kV, such as 16kV, 17kV, 20kV, 30kV, 40kV, 50kV, 60kV, 70kV, etc., preferably 15-18 kV.
Preferably, the spinning pitch of said electrospinning is from 10 to 40cm, such as 11cm, 12cm, 13cm, 14cm, 16cm, 18cm, 20cm, 22cm, 24cm, 26cm, 28cm, 30cm, 32cm, 34cm, 36cm, 38cm and the like, preferably from 12 to 15 cm.
Preferably, the liquid supply rate of the single spinneret flow channel for electrospinning is 0.5-2mL/h, such as 0.61mL/h, 0.62mL/h, 0.63mL/h, 0.64mL/h, 0.65mL/h, 0.66mL/h, 0.67mL/h, 0.68mL/h, 0.69mL/h, 0.7mL/h, 0.8mL/h, 0.9mL/h, 1mL/h, 1.2mL/h, 1.4mL/h, 1.6mL/h, 1.8mL/h, etc., preferably 0.6-0.7 mL/h.
Preferably, the electrospinning needle head slides at a speed of 15 to 30nm/s, for example, 16nm/s, 17nm/s, 18nm/s, 19nm/s, 20nm/s, 21nm/s, 22nm/s, 23nm/s, 24nm/s, 25nm/s, 26nm/s, 27nm/s, 28nm/s, 29nm/s, etc.
Preferably, the receiving roller speed of the electrostatic spinning is 80-200r/min, such as 90r/min, 100r/min, 110r/min, 120r/min, 130r/min, 140r/min, 150r/min, 160r/min, 170r/min, 180r/min, 190r/min and the like.
In the preferred technical scheme of the invention, the process conditions of electrostatic spinning are optimized, so that the filtering efficiency of the nanofiber membrane on aerosol is improved, and the filtering resistance is reduced.
Preferably, the preparation method specifically comprises: the electret nano-particles and ZnAc 2H are contained2Performing electrostatic spinning on the spinning solution of O and polymer to obtain the nanofiber filtering membrane on a receiving substrate;
the electrostatic spinning conditions were as follows: the temperature is 25 ℃, the humidity is 50%, the voltage is 15-80kV, the spinning distance is 10-40cm, and the liquid supply speed of a single spinning nozzle flow passage is 0.5-2 ml/h.
Preferably, the preparation method further comprises: and carrying out heat treatment on the nanofiber filtering membrane.
Preferably, the method of heat treatment comprises a thermal compounding process.
Preferably, the heat treatment temperature is 80-200 ℃, such as 90 ℃, 100 ℃, 110 ℃, 120 ℃, 130 ℃, 140 ℃, 150 ℃, 160 ℃, 170 ℃, 180 ℃, 190 ℃ and the like.
The invention also provides the application of the nanofiber filtering membrane in the mask, the protective clothing, the air purifier filtering membrane or the air conditioner filtering membrane.
The nanofiber filtering membrane provided by the invention can efficiently capture aerosol with a small diameter, has low filtration resistance and excellent antibacterial performance, can efficiently capture aerosol when being applied to the nanofiber filtering membranes such as masks and protective clothing, can block the infection of bacteria and viruses, and can not cause the problems of unsmooth breathing, sultriness and the like caused by wearing.
It is a fourth object of the present invention to provide a filter material comprising the nanofiber filtration membrane according to one of the objects and a first substrate provided on one side of the nanofiber filtration membrane.
Preferably, the first substrate includes any one of a polypropylene spunbonded nonwoven fabric, a polypropylene meltblown nonwoven fabric, a polyethylene terephthalate meltblown nonwoven fabric, a natural fiber woven fabric and knitted fabric, a chemical fiber woven fabric and knitted fabric, and a blended woven fabric and knitted fabric.
Preferably, the nanofiber filtration membrane further comprises a second substrate disposed on a side of the nanofiber filtration membrane remote from the first substrate.
Preferably, the second substrate includes any one of a fiber honeycomb network, a polypropylene spunbonded nonwoven fabric, a polypropylene melt-blown nonwoven fabric, a polyethylene terephthalate melt-blown nonwoven fabric, a natural fiber woven fabric and knitted fabric, a chemical fiber woven fabric and knitted fabric, and a blended woven fabric and knitted fabric.
Preferably, the filter material has a filtration efficiency for aerosols of > 91%, e.g., 91.37%, 92.2%, 93.2%, 95%, 99.155%, 99.8%, etc.
Preferably, the filter material has a gas resistance < 150Pa, such as 100Pa, 102Pa, 115Pa, 145Pa, and the like.
Compared with the prior art, the invention has the following beneficial effects:
the nanofiber filtering membrane provided by the invention simultaneously contains electret nanoparticles and ZnAc & 2H2And the O have synergistic effect, can effectively capture aerosol particles in the air, has lower filtration resistance, excellent antibacterial performance and self-cleaning performance, and is particularly suitable to be used as a filter material of protective articles such as masks, protective clothing and the like.
Drawings
FIG. 1 is an SEM test chart of a nanofiber filtration membrane in example 1 of the present invention.
FIG. 2 is an SEM test chart of a nanofiber filtration membrane in example 2 of the present invention.
FIG. 3 is an SEM test chart of a nanofiber filtration membrane of example 3 of the present invention.
FIG. 4 is a bacteriostatic performance test chart of the nanofiber filtration membrane in example 1 of the present invention.
Detailed Description
For the purpose of facilitating an understanding of the present invention, the present invention will now be described by way of examples. It should be understood by those skilled in the art that the examples are only for the understanding of the present invention and should not be construed as the specific limitations of the present invention.
In the specific embodiment of the invention, the method for testing the filtration efficiency and the air resistance comprises the following steps:
the method for testing the filtering efficiency comprises the following steps: the air carrying particles passes through the filter material, and the ratio of the difference value of the amount of the particles in the air at the air outlet to the amount of the particles in the air at the air inlet is obtained.
Testing air resistance: during the process of testing the filter material, the pressure difference between the pressure of the air inlet and the pressure of the air outlet is measured.
Example 1
The embodiment provides a nanofiber filter membrane, and a preparation method thereof comprises the following steps:
preparing a nanofiber filtering membrane: weighing SiO2Slowly adding into Dimethylformamide (DMF), and placing in ultrasonic cleaner for 1h to make SiO2Uniformly dispersing, adding PVDF powder with molecular weight of 200000, placing on a thermomagnetic stirrer, heating to 50 deg.C, stirring for more than 2 hr until PVDF is completely dissolved, and weighing ZnAc 2H2Adding O, and stirring under thermomagnetic force to obtain PVDF + SiO2(5％)+ZnAc·2H2O (5%) solution (percentages stand for SiO)2Is 5 percent, ZnAc 2H2The mass percentage of O is 10%). Adopting an electrostatic spinning method to obtain PVDF + SiO2+ZnAc·2H2Filling the O spinning solution into an injector, using PP non-woven fabric as a receiving base material, applying 18kV high voltage in an environment with the temperature of 25 ℃ and the humidity of 50%, adjusting the spinning space to be 15cm, the liquid supply speed to be 0.7mL/h, and the needle head sliding speed from side to sideThe temperature is 15nm/s, the rotating speed of a receiving roller is 120r/min, and after spinning is finished, thermal compounding treatment is carried out at the temperature of 90 ℃ to prepare the nanofiber filtering membrane (the SEM test result is shown in figure 1).
The experiment results of tests on the nanofiber filtering membrane show that the aerosol filtering efficiency is 91.37% and the air resistance is 102 Pa.
The relationship between the growth of bacteria in 2 bacterial suspensions after the nanofiber filtration membrane was added and the culture time was also studied with respect to the nanofiber filtration membrane, and the results are shown in fig. 4, compared with the growth of bacteria in bacterial suspensions to which no anti-nanofiber membrane was added.
As can be seen from fig. 4, the e.coli and s.aureus bacterial suspensions without the anti-nanofiber membrane added had a gradual increase in absorbance after 2 hours and a gradual stabilization in absorbance after 10 hours, indicating that the growth and reproduction of bacteria were normal in both bacterial suspensions. The suspensions of e.coli and s.aureus bacteria to which the nanofiber filtration membrane of example 1 was added did not show a gradual increase in absorbance, and were always in a steady state from the start to the end of the detection, indicating that the nanofiber filtration membrane plays a role in inhibiting the growth and reproduction of e.coli and s.aureus bacteria in the suspensions of e.coli and s.aureus.
Example 2
The difference from example 1 is only that SiO is present in the spinning solution2And ZnAc 2H2The mass ratio of O is different, specifically PVDF + SiO2(5％)+ZnAc·2H2O (10%), SEM test results of nanofiber filtration membrane are shown in fig. 2.
The experiment results of tests on the nanofiber filtering membrane show that the aerosol filtering efficiency is 93.2% and the air resistance is 115 Pa.
Example 3
The difference from example 1 is only that SiO is present in the spinning solution2And ZnAc 2H2The mass ratio of O is different, specifically PVDF + SiO2(5％)+ZnAc·2H2O (20%), SEM test results of nanofiber filtration membrane are shown in fig. 3.
The experiment results of tests on the nanofiber filtering membrane show that the aerosol filtering efficiency is 95% and the air resistance is 145 Pa.
Example 4
The embodiment provides a nanofiber filter membrane, and a preparation method thereof comprises the following steps:
preparing a nanofiber filtering membrane: weighing SiO2Slowly adding into Dimethylformamide (DMF), and placing in ultrasonic cleaner for 1h to make SiO2Uniformly dispersing, adding PVDF powder with molecular weight of 200000, placing on a thermomagnetic stirrer, heating to 50 deg.C, stirring for more than 2 hr until PVDF is completely dissolved, and weighing ZnAc 2H2Adding O, and stirring under thermomagnetic force to obtain PVDF + SiO2(5％)+ZnAc·2H2O (5%) solution (percentages stand for SiO)2Is 5 percent, ZnAc 2H2The mass percentage of O is 10%). Adopting an electrostatic spinning method to obtain PVDF + SiO2+ZnAc·2H2Filling the O spinning solution into an injector, taking PP non-woven fabric as a receiving base material, applying 15kV high voltage in an environment with the temperature of 25 ℃ and the humidity of 40%, adjusting the spinning space to be 12cm, the liquid supply speed to be 0.6mL/h, the left-right sliding speed of a needle head to be 30nm/s, the rotating speed of a receiving roller to be 100r/min, and after spinning is finished, carrying out thermal compounding treatment at the temperature of 100 ℃ to prepare the nanofiber filtering membrane.
The experiment results of tests on the nanofiber filtering membrane show that the aerosol filtering efficiency is 92.2 percent, and the air resistance is 100 Pa.
Example 5
The embodiment provides a nanofiber filter membrane, and a preparation method thereof comprises the following steps:
preparing a nanofiber filtering membrane: weighing SiO with corresponding mass2Slowly adding into Dimethylformamide (DMF), and placing in ultrasonic cleaner for 1h to make SiO2Uniformly dispersing, adding PVDF powder with molecular weight of 200000, placing on a thermomagnetic stirrer, heating to 50 deg.C, stirring for more than 2 hr until PVDF is completely dissolved, and weighing ZnAc 2H2Adding O, and stirring under thermomagnetic force to obtain PVDF + SiO2(5％)+ZnAc·2H2O (5%) solution (percentages stand for SiO)2Is 5 percent, ZnAc 2H2The mass percentage of O is 10%). Using static electricityThe spinning method comprises the steps of taking PVDF + SiO2+ZnAc·2H2Filling the O spinning solution into an injector, taking PET non-woven fabric as a receiving base material, applying 15kV high voltage in an environment with the temperature of 25 ℃ and the humidity of 50%, adjusting the spinning space to be 12cm, the liquid supply speed to be 0.6mL/h, the left-right sliding speed of a needle head to be 30nm/s, the rotating speed of a receiving roller to be 100r/min, and after spinning is finished, carrying out thermal compounding treatment at the temperature of 150 ℃ to prepare the nanofiber filtering membrane.
The experiment results of tests on the nanofiber filtering membrane show that the aerosol filtering efficiency is 89% and the air resistance is 85 Pa.
Comparative example 1
This comparative example provides a nanofiber filtration membrane, the preparation method of which differs from example 1 only in that no SiO is added2ZnAc 2H in spinning solution2The mass percentage of O is 10 percent, and the rest steps are the same.
The experiment results of tests on the nanofiber filtering membrane show that the aerosol filtering efficiency is 91%, the air resistance is 183Pa, and the nanofiber filtering membrane has a bacteriostatic effect.
Comparative example 2
This comparative example provides a nanofiber filtration membrane whose preparation process differs from that of example 1 only in that ZnAc 2H was not added2O, SiO in spinning solution2The mass percentage of (A) is 10%, and the rest steps are the same.
The experiment results of the tests on the nanofiber filtering membrane show that the aerosol filtering efficiency is 89%, the air resistance is 100Pa, and the nanofiber filtering membrane has no bacteriostatic effect.
The experimental results of the above examples and comparative examples demonstrate that electret nanoparticles and ZnAc 2H are simultaneously incorporated into polymer fibers2And the two are synergistic, so that the filtering efficiency can be effectively improved and the filtering resistance can be reduced compared with the case of only using one of the two.
The applicant states that the present invention is illustrated in detail by the above examples, but the present invention is not limited to the above detailed methods, i.e. it is not meant that the present invention must rely on the above detailed methods for its implementation. It should be understood by those skilled in the art that any modification of the present invention, equivalent substitutions of the raw materials of the product of the present invention, addition of auxiliary components, selection of specific modes, etc., are within the scope and disclosure of the present invention.

Claims (10)

1. A nanofiber filtration membrane comprising polymer fibers and electret nanoparticles and ZnAc 2H attached to the surfaces of the polymer fibers2O。
2. The nanofibrous filtration membrane according to claim 1, characterized in that the electret nanoparticles comprise any one or a combination of at least two of silica, Zif-8, tetraoxyethylene, boehmite, barium titanate or silicon nitride, preferably silica.
3. The nanofibrous filtration membrane according to claim 1 or 2, characterized in that the polymer fibers comprise any one or a combination of at least two of polyvinyl chloride fibers, polyacrylonitrile fibers, polyethersulfone fibers, polyurethane fibers, polyvinyl alcohol fibers or polyvinylpyrrolidone fibers.
4. Nanofibrous filtration membrane according to any one of claims 1 to 3, characterised in that the electret nanoparticles and ZnAc-2H2The mass ratio of O is 1 (0.2-10).
5. The nanofibrous filtration membrane according to any of claims 1 to 4, characterized by an efficiency > 93% for aerosol filtration;
preferably, the nanofiber filtration membrane has an air resistance < 385 Pa.
6. The nanofiber filtration membrane manufacturing method according to any one of claims 1 to 5, comprising: the electret nano-particles and ZnAc 2H are contained2O and polymer spinning solutionAnd (3) carrying out electrostatic spinning to obtain the nanofiber filtering membrane on a receiving substrate.
7. The production method according to claim 6, wherein ZnAc-2H in the spinning solution2The mass percentage of O is 5-20%;
preferably, in the spinning solution, the mass percentage of the electret nanoparticles is 1% -30%, preferably 5%;
preferably, the receiving substrate comprises any one of polypropylene spunbonded non-woven fabric, polypropylene melt-blown non-woven fabric, polyethylene terephthalate melt-blown non-woven fabric, natural fiber woven fabric and knitted fabric, chemical fiber woven fabric and knitted fabric, and blended woven fabric and knitted fabric;
preferably, the polymer comprises any one or a combination of at least two of polyvinyl chloride, polyacrylonitrile, polyethersulfone, polyurethane, polyvinyl alcohol, or polyvinylpyrrolidone.
8. The method of manufacturing according to claim 6 or 7, wherein the temperature of the electrospinning is 20 to 30 ℃, preferably 25 ℃;
preferably, the moisture of the electrospinning is 40% -60%, preferably 50%;
preferably, the voltage of the electrostatic spinning is 15-80 kV;
preferably, the spinning distance of the electrostatic spinning is 10-40 cm;
preferably, the liquid supply speed of a single spinning nozzle flow passage for electrostatic spinning is 0.5-2 ml/h;
preferably, the preparation method specifically comprises: the electret nano-particles and ZnAc 2H are contained2Performing electrostatic spinning on the spinning solution of O and polymer to obtain the nanofiber filtering membrane on a receiving substrate;
the electrostatic spinning conditions were as follows: the temperature is 25 ℃, the humidity is 50%, the voltage is 15-80kV, the spinning distance is 10-40cm, and the liquid supply speed of a single spinning nozzle flow channel is 0.5-2 ml/h;
preferably, the preparation method further comprises: heat treating the nanofiber filtration membrane;
preferably, the method of heat treatment comprises a thermal compounding treatment;
preferably, the temperature of the heat treatment is 80 to 200 ℃.
9. Use of a nanofibre filtration membrane according to any of claims 1 to 5 in a mask, a protective clothing, an air purifier filtration membrane or an air conditioner filtration membrane.
10. A filter material, comprising the nanofiber filtration membrane of any one of claims 1 to 5 and a first substrate disposed on one side of the nanofiber filtration membrane;
preferably, the first substrate comprises any one of polypropylene spunbonded non-woven fabric, polypropylene melt-blown non-woven fabric, polyethylene terephthalate melt-blown non-woven fabric, natural fiber woven fabric and knitted fabric, chemical fiber woven fabric and knitted fabric, and blended woven fabric and knitted fabric;
preferably, the nanofiber filtration membrane further comprises a second substrate disposed on a side of the nanofiber filtration membrane remote from the first substrate;
preferably, the second substrate comprises any one of a fiber honeycomb network, a polypropylene spunbonded non-woven fabric, a polypropylene melt-blown non-woven fabric, a polyethylene terephthalate melt-blown non-woven fabric, a natural fiber woven fabric and knitted fabric, a chemical fiber woven fabric and knitted fabric, and a blended woven fabric and knitted fabric;
preferably, the filter material has an aerosol filtration efficiency of > 91%;
preferably, the filter material has a gas resistance of < 150 Pa.
CN202110929883.4A 2021-08-13 2021-08-13 Nanofiber filtering membrane and preparation method and application thereof Pending CN113457477A (en)

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