WO2017007267A1 - Procédé de préparation d'un filtre de nanofibres fonctionnelles, et filtre de nanofibres fonctionnelles ainsi préparé - Google Patents

Procédé de préparation d'un filtre de nanofibres fonctionnelles, et filtre de nanofibres fonctionnelles ainsi préparé Download PDF

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Publication number
WO2017007267A1
WO2017007267A1 PCT/KR2016/007397 KR2016007397W WO2017007267A1 WO 2017007267 A1 WO2017007267 A1 WO 2017007267A1 KR 2016007397 W KR2016007397 W KR 2016007397W WO 2017007267 A1 WO2017007267 A1 WO 2017007267A1
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nanofiber filter
functional
filter
nanofiber
nanomaterial
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PCT/KR2016/007397
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English (en)
Korean (ko)
Inventor
최희철
배지열
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광주과학기술원
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Publication of WO2017007267A1 publication Critical patent/WO2017007267A1/fr

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D39/00—Filtering material for liquid or gaseous fluids
    • B01D39/14—Other self-supporting filtering material ; Other filtering material
    • B01D39/16—Other self-supporting filtering material ; Other filtering material of organic material, e.g. synthetic fibres
    • D—TEXTILES; PAPER
    • D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
    • D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
    • D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
    • D04H1/42—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties characterised by the use of certain kinds of fibres insofar as this use has no preponderant influence on the consolidation of the fleece
    • D—TEXTILES; PAPER
    • D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
    • D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
    • D04H1/70—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres
    • D04H1/72—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres the fibres being randomly arranged
    • D04H1/728—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres the fibres being randomly arranged by electro-spinning

Definitions

  • the present invention relates to a nanofiber filter, and more particularly to a method for producing a nanofiber filter comprising a functional nanomaterial and a functional nanofiber filter produced thereby.
  • the filter includes one or more nanofibers in the form of a web with substrate material in the filter structure.
  • the nanofibers are fibers of several hundred nanometers (nm) or less in diameter, and refer to a new concept of fiber material having different functions and performances from existing fiber materials. Since the nanofibers contain a plurality of pores, the nanofiber filters including these nanofibers can separate dozens of nano-sized particles or more, purifying large amounts of water or removing particulates in the air in a short time. It has good filtration and high particle trapping ability to filter effectively.
  • the conventional nanofiber filter used in water treatment has a problem that the separation efficiency is significantly reduced as the surface of the nanofiber filter is contaminated by microorganisms to be separated for a long time, thereby increasing energy consumption and filter consumption.
  • Such functional nanofibers are mainly used to prepare a mixture in which a functional material is added to a nanofiber constituent material into nanofibers in a web form.
  • the nanofibers produced by this manufacturing method are difficult to uniformly disperse the functional material on the surface, and the functional material mixed in the nanofiber constituent material affects the size of the pores of the nanofiber filter, thereby degrading the separation performance of the filter. There are disadvantages.
  • An object of the present invention is to provide a method for producing a functional nanofiber filter and a nanofiber filter produced thereby, which can efficiently fix various functional nanomaterials to a nanofiber filter.
  • an aspect of the present invention includes the steps of preparing a spinning solution by adding a polysulfone polymer to an organic solvent, forming a nanofiber filter by electrospinning the spinning solution, and a functional nanomaterial dispersion solvent. After dipping the nanofiber filter to dry, it can provide a method for producing a functional nanofiber filter comprising the step of attaching the functional nanomaterial to the nanofiber filter.
  • the polysulfone polymer may be any one selected from polysulfone, polyethersulfone, and mixtures thereof.
  • the organic solvent is N-methyl-2-pyrrolidone (N-methyl-2-pyrrolidone, NMP), dimethylformamide (dimethylformamide, DMF), chloroform, dimethyl sulfoxide (dimethylsulfoxide) and N, N- It may be at least one selected from dimethylacetamide (N, N-dimethylacetamide, DMAc).
  • the polysulfone polymer may be added in an amount of 25 to 40 wt% based on the organic solvent.
  • the applied voltage may be 8 to 13 kV.
  • the discharge rate of the spinning solution may be 0.1 to 2mL / hr.
  • the spinning distance may be 10 to 25cm.
  • the functional nanomaterial dispersion solvent is Ag, Be, Mg, Al, V, Cr, Mn, Fe, Co, Ni, Zn, Ga, Se, Cd, In, Sn, Te, Au, Pb, Bi, TiO 2 , At least one selected from SnO 2 , In 2 O 3 , Al 2 O 3 , SnO 2 , MnO 2 ZnO, WO 3 , carbon nanotubes, graphene and nano clays It may include a functional nanomaterial of.
  • the functional nanomaterial may be attached to the surface of the nanofiber filter as the nanofiber filter is solidified.
  • another aspect of the present invention can provide a functional nanofiber filter prepared through the method for producing the functional nanofiber filter.
  • the manufacturing method of the functional nanofiber filter of the present invention can easily attach the nanomaterial having the functionalities to the surface of the nanofiber, and can produce a nanofiber filter having various functions even with a simple process.
  • the nanofiber filter is manufactured using the electrospinning method, the thickness of the thin film and the size of the pores can be easily adjusted, and thus have high porosity and excellent mechanical strength.
  • the silver (Ag) nanomaterial may have an antibacterial function, it is possible to improve the filter contamination problem by the conventional microorganisms, and to reduce the energy and filter consumption.
  • FIG. 1 is a flow chart for explaining a method of manufacturing a functional nanofiber filter according to an embodiment of the present invention.
  • FIG 2 is an image showing an electrospinning apparatus according to an embodiment of the present invention.
  • Example 3 is an image showing the surface characteristics of the nanofiber filter prepared in Example 1 and Comparative Example 1 of the present invention.
  • Figure 4 is an image showing the microbial culture test results of the nanofiber filter of Example 1 and Comparative Examples 1 to 2 of the present invention.
  • FIG. 1 is a flow chart for explaining a method of manufacturing a functional nanofiber filter according to an embodiment of the present invention.
  • a polysulfone polymer may be added to an organic solvent to prepare a spinning solution (S100).
  • the polysulfone polymer may be a polysulfone polymer having a unit of an aryl (Aryl) group and a sulfate group as a main material of the nanofiber filter of the present invention.
  • the polysulfone polymer may be any one selected from polysulfone, polyethersulfone, and mixtures thereof.
  • the organic solvent is N-methyl-2-pyrrolidone (N-methyl-2-pyrrolidone, NMP), dimethylformamide (dimethylformamide, DMF), chloroform (chloroform), dimethyl sulfoxide (dimethylsulfoxide) and N, N-dimethylacetamide (N, N-dimethylacetamide, DMAc) may be at least one selected from.
  • N-methyl-2-pyrrolidone (NMP) has a high viscosity compared to other solvents has a low volatility, it can be used to improve the mechanical strength of the polysulfone polymer.
  • N-methyl-2-pyrrolidone (NMP) may be used as the organic solvent, but is not limited thereto.
  • the polysulfone polymer may be added in an amount of 25 to 40 wt% based on the organic solvent.
  • the polysulfone-based polymer When the polysulfone-based polymer is added in less than 25% by weight with respect to the organic solvent, it may be difficult to form nanofibers having a uniform diameter or do not form nanofibers because spinning does not proceed smoothly.
  • the polysulfone-based polymer when the polysulfone-based polymer is added in excess of 40% by weight relative to the organic solvent, the viscosity of the mixed spinning solution is rapidly increased and spinning may not be performed or processability may be lowered.
  • a nanofiber filter may be formed by electrospinning the spinning solution prepared in step S100 (S200).
  • the spinning solution may be formed in the form of nanofibers having a diameter of a nano size using an electrospinning apparatus.
  • a plurality of nanofibers formed by using an electrospinning process are concentrated into nanofiber aggregates in the form of a web, and the nanofiber aggregates can be used as nanofiber filters requiring high porosity and three-dimensional structure.
  • an electrospinning apparatus as shown in FIG. 2 may be used to perform the electrospinning process.
  • the spinning solution may be discharged through the spinning nozzle of the device while supplying the spinning solution in a predetermined amount using the metering pump of the device.
  • the discharged spinning solution may be formed of nanofibers solidified at the same time as scattering and concentrated in a collector to form a nanofiber aggregate.
  • the diameter of the nanofibers constituting the nanofiber filter may be 400nm to 600nm, but is not limited thereto.
  • the voltage When performing the electrospinning, the voltage may be 8 to 13kV. When the intensity of the applied voltage is 8 kV or less, the radiation of the spinning solution may not occur. When the intensity of the applied voltage is 13 kV or more, the spinning solution is spun in a spray form to form nanofibers. May be inhibited.
  • the discharge rate of the spinning solution may be 0.1 to 2mL / hr.
  • the discharge rate of the spinning solution is less than 0.1mL / hr, the spinning solution is not continuously discharged, it is not possible to form a nanofiber of uniform size.
  • the discharge rate of the spinning solution exceeds 2mL / hr, some of the discharged spinning solution is not collected in the collector can reduce the productivity.
  • the spinning distance When performing the electrospinning, the spinning distance may be 10 to 25cm.
  • the radiation distance may mean a distance between the radiator and the collector of the electrospinning apparatus. If the spinning distance is less than 10cm, the scattering time of the spinning solution may be reduced to obtain a solidified nanofibers. In addition, when the spinning distance is more than 25cm, the homogeneity of the nanofibers may be reduced.
  • the temperature may be 20 to 30.
  • the nanofiber may not be formed when the composition temperature during the electrospinning is less than 20, and the strength of the nanofiber filter formed by completely volatilizing the solvent may be weakened when the composition temperature during the electrospinning is greater than 30. have.
  • the nanofibers electrospun in S200 may be immersed in a functional nanomaterial dispersion solvent and dried to attach the functional nanomaterial to the nanofiber filter (S300). Specifically, in step S300, as the nanofiber filter is solidified, the functional nanomaterial may be attached to the surface of the nanofiber filter. This will be described in detail below.
  • the organic solvent contained in the spinning solution remains. By this remaining organic solvent, the electrospun nanofiber filter cannot be completely solidified.
  • the present invention by immersing the electrospun nanofiber filter is not completely solid as described above in the functional nanomaterial dispersion solvent and dried, the nanofiber filter is not completely volatilized during the scattering period of the electrospinning step of step S200
  • the organic solvent remaining in the substrate may be removed and the electrospun nanofiber filter may be solidified, and the functional nanomaterial may be attached by using the phenomenon in which the nanofiber filter is solidified.
  • the nanofiber filter is immersed in the functional nanomaterial dispersion solvent to arrange the functional nanomaterial on the surface of the nanofiber filter, and the electrospun nanofiber filter is solidified. While solidifying, the functional nanomaterial may be physically attached to the surface of the nanofiber filter. This is to improve the process of removing and solidifying the remaining organic solvent by dipping the conventional electrospun nanofiber filter in distilled water, the present invention effectively removes the organic solvent to solidify the nanofiber filter, The functional nanomaterial may be immobilized on the surface of the nanofiber filter without an adhesion process or an application process, thereby improving manufacturing process efficiency.
  • a functional nanomaterial dispersion solvent may be prepared.
  • the functional nanomaterial dispersion solvent refers to a solvent in which the functional nanomaterial is dispersed, and the functional nanomaterial may use all materials having various functionalities.
  • the solvent included in the functional nanomaterial dispersion solvent any known solvent capable of uniformly dispersing the functional nanomaterial may be used without affecting the functional nanomaterial.
  • the solvent may vary depending on the type of the functional nanomaterial, and is not particularly limited.
  • the functional nanomaterial dispersion solvent is silver (Ag), beryllium (Be), magnesium (Mg), aluminum (Al), vanadium (V), chromium (Cr), manganese (Mn), iron (Fe), cobalt (Co) ), Nickel (Ni), zinc (Zn), gallium (Ga), ceryllium (Se), cadmium (Cd), indium (In), tin (Sn), teryllium (Te), gold (Au), lead (Pb), bismuth (Bi), titanium dioxide (TiO 2 ), tin oxide (SnO 2 ), indium oxide (In 2 O 3 ), aluminum oxide (Al 2 O 3 ), manganese oxide (MnO 2 ), zinc oxide (ZnO), tungsten oxide (WO 3 ), carbon nanotubes (carbon nanotube), graphene (graphene) and nanoclays (nano clay) may include at least one functional nanomaterial selected from.
  • the above-described functional nanomaterials have various characteristics
  • the silver (Ag) nanomaterial has an antibacterial function of killing bacteria by inhibiting enzymes that control the respiration of bacteria when silver (Ag) ions come into contact with the bacteria, and oxidation of silver (Ag). It has sterilizing function due to active oxygen produced by the action.
  • silver (Ag) nanoparticles are immobilized on the surface of the nanofiber filter using the antibacterial and sterilizing function of silver (Ag), thereby preventing contamination of the surface of the nanofiber filter.
  • the titanium dioxide (TiO 2 ) nanomaterial has a large oxidizing power, can act as antibacterial, odor removal and sterilization, and can absorb ultraviolet light to serve as a photocatalyst.
  • the present invention can improve the performance of the nanofiber filter using the photocatalytic function, antibacterial and sterilization function of the titanium dioxide (TiO 2 ), it is possible to reduce the filter consumption.
  • Immersion time may be 1 hour to 2 hours.
  • the functional nanomaterial may not be uniformly dispersed on the nanofiber filter surface.
  • the immersion time exceeds 2 hours, the shape of the electrospun nanofiber filter of the web structure can be modified, it is possible to perform the immersion process within the time range.
  • a dispersion solvent containing silver (Ag) nanomaterial may be used, but is not limited thereto.
  • the dispersion solvent containing the silver (Ag) nanomaterial is mixed with a silver (Ag) aqueous solution and a reducing agent containing silver (Ag) ions capable of providing the silver (Ag) nanomaterial. It may have been.
  • the silver (Ag) aqueous solution may be at least one selected from silver nitrate (AgNO 3 ), silver chloride (AgCl), silver sulfide (Ag 2 S), and silver acetate (CH 3 COOAg), but is not limited thereto.
  • the reducing agent may serve to reduce the silver (Ag) ions contained in the aqueous solution.
  • the reducing agent may be at least one selected from hydrazine (N 2 H 4 ), sodium borohydride (NaBH 4 ), and formaldehyde (HCHO), but is not limited thereto.
  • the silver (Ag) nanomaterial dispersion solvent may be a mixture of sodium borohydride (NaBH 4 ) and silver nitrate (AgNO 3 ) in a volume ratio of 3: 1.
  • the concentration of NaBH 4 may be 0.02M
  • the concentration of AgNO 3 may be 0.01M, but is not limited thereto.
  • the process of mixing the silver (Ag) aqueous solution and the reducing agent may be performed at a temperature of about 0, and by injecting a drop of the silver (Ag) aqueous solution into the reducing agent solution in about one second to mix silver (Ag )
  • the nanomaterial dispersion solvent can be prepared.
  • the manufacturing method of the functional nanofiber filter of the present invention uses the electrospinning process to produce a nanofiber filter having a high porosity, and the nanofiber filter functional nanomaterial during the process of solidifying the nanofiber filter
  • the functional nanomaterial can be easily attached to the nanofiber filter by contact with a dispersion solvent.
  • the functional nanomaterial which is physically immobilized on the surface of the nanofiber filter in the process of solidification, has excellent adhesion and does not require a separate bonding process, thereby improving manufacturing process efficiency and reducing manufacturing cost.
  • the functional nanofiber filter is made of a polysulfone-based polymer, and may be manufactured by electrospinning to have a higher porosity than conventional environmental purification filters.
  • the functional nanofiber filter may be given various functions due to the characteristics of the functional nanomaterial as the functional nanomaterial is immobilized on the surface of the nanofiber. For example, when attaching a functional nanomaterial having antimicrobial and bactericidal functions to the functional nanofiber filter, it is possible to improve the problem of the prior art that the filter surface was contaminated by microorganisms when used for water treatment applications.
  • it can be used as a filter having excellent breathability even when used for air purification applications, it can be utilized as an antibacterial filter, it is expected that the application field will be expanded.
  • a commercially available polyethersulfone polymer was dissolved in a 30% weight ratio of N-methyl-2-pyrrolidone (NMP) solvent to prepare a spinning solution. This was discharged through a syringe (syringe) installed in the electrospinning apparatus as shown in FIG. 2 through a metering pump, and then scattered in a state where an electric field was applied by a high voltage generator to form a coagulated nano-sized fiber.
  • the nanofiber filter formed of polyether sulfone was prepared by focusing the nanofibers formed and solidified in the collector. At this time, the applied voltage was 13 kW, the radiation distance was 20 cm, the temperature and humidity at the time of spinning were 25 to 30 ?, respectively, and the relative humidity was 40 to 45%.
  • silver (Ag) nanomaterials were used as functional nanomaterial dispersion solvents.
  • NaBH 4 solution and AgNO 3 solution was mixed in a volume ratio of 3: 1 to prepare a silver (Ag) nanomaterial dispersion solvent.
  • the polyether sulfone nanofiber filter was immersed in a silver (Ag) nanomaterial dispersion solvent to coagulate, and then dried in air to prepare a nanofiber filter.
  • Nanofiber filters were prepared.
  • a commercially available 0.45 ⁇ m nylon (nylon) filter manufactured by Millipore was prepared.
  • the components of the nanofiber filters prepared in Example 1 and Comparative Example 1 were analyzed. Specifically, surface analysis of the nanofiber filter was performed using a scanning electron microscope (SEM) -energy dispersive X-ray analyzer (EDX), and energy dispersive x-ray spectroscopy (EDS). The component analysis of the filter was performed using.
  • SEM scanning electron microscope
  • EDX energy dispersive X-ray analyzer
  • EDS energy dispersive x-ray spectroscopy
  • Example 3 is an image showing the surface characteristics of the nanofiber filter prepared in Example 1 and Comparative Example 1 of the present invention.
  • Example 2 In order to compare and analyze membrane performance of the nanofiber filters prepared in Example 1 and Comparative Example 1, their contaminant removal efficiency was analyzed. Specifically, the influent used in the pollutant removal experiment was prepared by using a turbidity solution of 100NTU according to the microfiltration membrane module and ultrafiltration membrane module test method for water. At this time, the turbidity causing material used was Kaolin (Sigma-aldrich), the performance evaluation results are shown in Table 2 below.
  • the functional nanofiber filter of the present invention does not significantly affect the filtration performance of the silver (Ag) nanoparticles. That is, the functional nanofiber filter of the present invention can impart the functionality of the functional nanomaterial while maintaining the separation and filtration functions of the nanofiber filter, and can be actively utilized in various fields.
  • Figure 4 is an image showing the microbial culture test results of the nanofiber filter of Example 1 and Comparative Examples 1 to 2 of the present invention.
  • the microorganisms are clustered in the nanofiber filter to which silver (Ag) nanoparticles of Comparative Example 1 and Comparative Example 2 are not attached. It can be seen that the microbial community effect does not occur in the nanofiber filter to which silver (Ag) nanoparticles of Example 1 are attached.
  • the nanofiber filter of Example 1 of the present invention can be confirmed that the microbial community effect does not occur continuously after 5 days. Through this, it can be seen that the nanofiber filter with silver (Ag) nanoparticles of the present invention has an antibacterial function.

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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Filtering Materials (AREA)
  • Nonwoven Fabrics (AREA)

Abstract

L'invention concerne un procédé de préparation d'un filtre de nanofibres fonctionnelles, et un filtre de nanofibres fonctionnelles ainsi préparé. L'invention concerne plus particulièrement un filtre de nanofibres fonctionnelles que l'on peut préparer selon les étapes consistant à : préparer une solution de filage en ajoutant un solvant organique à un polymère à base de polysulfone ; former un filtre de nanofibres en soumettant la solution de filage à un filage électrostatique ; faire adhérer un nanomatériau fonctionnel au filtre de nanofibres, en immergeant le filtre de nanofibres dans le solvant de dispersion de nanomatériau fonctionnel, et ensuite sécher le filtre.
PCT/KR2016/007397 2015-07-08 2016-07-07 Procédé de préparation d'un filtre de nanofibres fonctionnelles, et filtre de nanofibres fonctionnelles ainsi préparé WO2017007267A1 (fr)

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KR10-2015-0096883 2015-07-08
KR1020150096883A KR101683475B1 (ko) 2015-07-08 2015-07-08 기능성 나노섬유 필터의 제조방법 및 이에 의해 제조된 기능성 나노섬유 필터

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KR102168209B1 (ko) * 2020-04-06 2020-10-20 이계영 마스크용 항균필터와 이의 제조방법 및 항균 마스크
KR102406893B1 (ko) 2021-12-16 2022-06-13 주식회사 서현어패럴 나노탄소섬유 신발 뒤꿈치용 패드 제조방법 및 그 패드
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KR101485119B1 (ko) * 2014-02-12 2015-01-22 광주과학기술원 전기방사를 이용한 개선된 폴리에테르설폰 나노섬유 멤브레인의 제조방법

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CN113782278A (zh) * 2021-09-16 2021-12-10 北京科技大学 一种纤维基各向异性可拉伸导体的制备方法
CN114471196A (zh) * 2021-12-20 2022-05-13 中国科学院新疆生态与地理研究所 一种多功能纳米纤维水净化膜的制备方法
CN114471196B (zh) * 2021-12-20 2023-11-14 中国科学院新疆生态与地理研究所 一种多功能纳米纤维水净化膜的制备方法

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