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WO2018208040A2 - Filtre de collecte de substances nocives hautes performances et son procédé de fabrication - Google Patents

Filtre de collecte de substances nocives hautes performances et son procédé de fabrication Download PDF

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Publication number
WO2018208040A2
WO2018208040A2 PCT/KR2018/005075 KR2018005075W WO2018208040A2 WO 2018208040 A2 WO2018208040 A2 WO 2018208040A2 KR 2018005075 W KR2018005075 W KR 2018005075W WO 2018208040 A2 WO2018208040 A2 WO 2018208040A2
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WIPO (PCT)
Prior art keywords
nanofibers
surface treatment
filter
treated
collection filter
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Ceased
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PCT/KR2018/005075
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English (en)
Korean (ko)
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WO2018208040A3 (fr
Inventor
김한중
박선주
권오석
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Korea Research Institute of Bioscience and Biotechnology KRIBB
Center for Integrated Smart Sensors Foundation
Original Assignee
Korea Research Institute of Bioscience and Biotechnology KRIBB
Center for Integrated Smart Sensors Foundation
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Publication of WO2018208040A2 publication Critical patent/WO2018208040A2/fr
Publication of WO2018208040A3 publication Critical patent/WO2018208040A3/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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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

Definitions

  • the present invention relates to a harmful substance collection filter and a method of manufacturing the same, and more particularly, to include a surface-treated nanofibers to improve chemical bonding between the target material and the nanofibers, and to reduce the flow of air according to the diameter reduction of the nanofibers.
  • the present invention relates to a filter that improves the ability to collect harmful substances by improving.
  • a filter is defined as a thin film that filters foreign matter in a liquid or gas.
  • the method of removing harmful substances including fine dust from the gas can be divided into electric dust collection type and dry and wet filter type.
  • Electrostatic precipitating is a method of adsorbing fine dust in the air to absorb dust using a force such as static electricity, and is selectively charged with (+) and (-) to attract and attract dust to a parallel and dense metal dust collecting plate. Accordingly, the collected fine dust is agglomerated into a mass by molecular cohesion.
  • the electrostatic precipitating method has an advantage in that the inside is simple, so there is little noise, and when a fan having the same capacity is used, the amount of air after the dust collection is large, and thus no need to replace the filter.
  • the metal dust collecting plate that collects dust should be cleaned periodically, and power must be supplied to have a dust collecting effect, and the installation space is large.
  • Dry filter is a method of filtering dust in the air like a filter paper using a cloth or paper containing a small hole.
  • the filter can be classified into a prefilter, a medium filter, a HEPA (0.3 micrometer), and a ULPA (0.12 micrometer) according to how small dust can be filtered out.
  • HEPA and ULPA filters are very small holes through which the air passes to filter out fine dust, but the power to pass through the air must be very large, which requires a large amount of power required, and glass fiber dust is generated when the filter is manufactured.
  • wet filter type sprays liquid such as water into small vapor as if spraying with sprayer to combine water droplets and dust to remove dust, or absorbs liquid such as water to filter to remove dust by contact with water and dust. That's the way it is.
  • the wet filter type has the disadvantage that the efficiency is low in the place where the air speed is fast.
  • Nanofiber based filters have the advantage that the specific surface area is very large and thin compared to the filter media of the existing filter having a large diameter, so that the pressure loss of air is small and flexible.
  • the nanofiber based filter has a limitation that it is difficult to control the conditions for production and performance improvement.
  • the prior art Korean Patent Publication No. 10-2011-0049952
  • a mixed catalyst filter having pores by secondary heat treatment has been described, this conventional technique has a disadvantage in that the manufacturing process is complicated and there is a limitation in that an additional catalyst is required.
  • An object of the present invention is to surface-treated on nanofibers to increase the chemical bonding force between the harmful substances (subject material) and nanofibers including fine dust and to improve the performance of the conventional nanofiber filter and a filter for collecting harmful substances and its preparation To provide a method.
  • an object of the present invention is to provide a harmful substance collection filter and a method for manufacturing the same that can ensure a smooth air-flow (air-flow) by reducing the diameter of the nanofiber by surface treatment on the nanofiber.
  • an object of the present invention is to provide a harmful material collection filter and a method for manufacturing the same, which can improve the collecting power by changing the physical and chemical structure of the nanofiber without using a catalyst by surface treatment on the nanofiber.
  • the method of manufacturing a noxious substance trap filter according to an embodiment of the present invention includes forming a nanofiber and surface treating the nanofiber to increase the chemical bonding force between the target material and the nanofiber, wherein the surface
  • the step of treating is characterized in that by inducing changes in the physical and chemical properties of the nanofibers to improve the capture power.
  • the method for manufacturing a harmful substance collection filter according to an embodiment of the present invention may further include applying the surface-treated nanofibers to the filter.
  • the surface treatment may increase the specific surface area and minimize the pressure loss of air by reducing the diameter of the nanofibers by surface treatment.
  • the surface treatment may induce a change in the characteristics of the nanofibers by treating the surface of the nanofibers with reactive ion etching (RIE).
  • RIE reactive ion etching
  • the surface treatment may be performed by surface treatment of the reactive ion etching to form an amide group (-CONH), ester group (-COOR) and carboxyl group (-COOH) on the nanofibers to increase the chemical bonding force according to the dipole moment increase Can be.
  • the surface treatment may improve the collection force due to an increase in the chemical bonding force between the target material and the nanofiber by adjusting the conditions of the surface treatment.
  • the surface treatment may induce a property change of the nanofibers by subjecting the nanofibers to the surface treatment of a thermal annealing process.
  • the surface treatment of the plasma coating may be induced on the nanofibers.
  • the surface treatment may induce a characteristic change of the nanofibers by treating the surface of a self-assembly monolayer (SAM) patterned on the nanofibers to form a plurality of lines.
  • SAM self-assembly monolayer
  • the surface treatment may induce a change in the properties of the nanofibers by the surface treatment of conductive nanoparticle coating or substitution on the nanofibers.
  • a noxious substance trap filter according to an embodiment of the present invention is a noxious substance trap filter including nanofibers, characterized in that it comprises the nanofiber surface treated to increase the chemical bonding force between the target material and the nanofibers. .
  • the surface-treated nanofibers may be reduced in diameter by the surface treatment to increase specific surface area, thereby minimizing air pressure loss.
  • the surface-treated nanofibers may be changed in physical and chemical properties by the surface treatment of reactive ion etching (RIE).
  • RIE reactive ion etching
  • the surface treated nanofibers may be changed in physical and chemical properties by the surface treatment of a thermal annealing process.
  • the surface-treated nanofibers may be changed in physical and chemical properties by the surface treatment of a plasma coating.
  • the surface-treated nanofibers may be patterned to change physical and chemical properties by the surface treatment of a self-assembly monolayer (SAM) forming a plurality of lines.
  • SAM self-assembly monolayer
  • the surface treated nanofibers may be changed in physical and chemical properties by the surface treatment of conductive nanoparticle coating or substitution.
  • Hazardous substance collection filter is characterized in that it comprises a filter surface-treated to increase the chemical bonding force with the target material.
  • an air purifying filter excellent in collecting power of harmful substances including fine dust and an air purifying device to which the air purifying filter is applied.
  • by surface treatment on the nanofibers can reduce the diameter of the nanofibers to ensure a smooth air-flow (air-flow).
  • the chemical bonding force with the harmful substances and the physical change due to the reduction of the diameter of the nanofibers to improve the trapping of harmful substances, and to reduce the diameter of the nanofibers It provides a smooth air flow (minimizing pressure loss) and can be expected to increase the life of the filter at the same time.
  • FIG. 1 is a flowchart illustrating a method of manufacturing a hazardous substance collection filter according to an exemplary embodiment of the present invention.
  • FIGS. 2A and 2B illustrate examples of nanofibers included in a hazardous substance collection filter according to an exemplary embodiment of the present invention.
  • FIG. 3 is a graph showing the performance change of the surface-treated nanofibers according to the embodiment of the present invention.
  • Figure 4 shows the image results for the characteristic change of the surface-treated nanofibers according to the embodiment of the present invention.
  • FIG. 5 shows the results of surface modified XPS data of surface treated nanofibers according to an embodiment of the present invention.
  • FIG 6 illustrates changes in contact angles of nanofibers before and after surface treatment according to an embodiment of the present invention.
  • Figure 7 shows the performance change of the filter comprising a surface treated nanofiber according to an embodiment of the present invention.
  • FIG. 1 is a flowchart illustrating a method of manufacturing a hazardous substance collection filter according to an exemplary embodiment of the present invention.
  • step 110 nanofibers are formed.
  • Nanofibers for example, are ultrafine yarns with diameters of only tens to hundreds of nanometers (nm), and can be used as filters because of their large surface area relative to their volume.
  • the material and type of the nanofibers are not limited.
  • the method for preparing a hazardous substance collecting filter according to an embodiment of the present invention may use a membrane or microfiber in a larger range than the nanofibers, but the present invention will focus on nanofibers.
  • step 110 is a method for forming nanostructured material by block segment, nanostructured material forming method by self-assembly, nanofiber forming method by polymerization using silica catalyst, melt spinning, solvent extraction spinning, nonwoven spinning, Nanofibers may be formed using at least one of a nanofiber forming method by air jet spinning, flash spinning and precursor-based gas phase growth methods, and a nanofiber forming method by electrospinning a polymer solution or a melt.
  • step 120 the nanofibers are surface treated to increase the chemical bonding force between the target material and the nanofibers.
  • step 120 induces a change in physical and chemical properties of the nanofibers to improve the capture power.
  • the method for manufacturing a hazardous material filter according to an embodiment of the present invention may increase the specific surface area by minimizing the diameter of the nanofiber by surface treatment and minimize the pressure loss of air to reduce the power required.
  • step 120 may be a step of surface treatment of reactive ion etching (RIE) on the nanofibers to induce a change in the properties of the nanofibers.
  • RIE reactive ion etching
  • the surface treatment of the reactive ion etching may form an amide group (-CONH), ester group (-COOR) and carboxyl group (-COOH) on the nanofibers to increase the chemical bonding force according to the increase in the dipole moment,
  • the collection force may be improved by increasing the chemical bonding force between the target material and the nanofibers.
  • the reactive ion etching (RIE) is carried out at 50 sccm, 50 W, 100 mtorr, 30 seconds to 1 cycle, 2 cycles and 3 cycles of processing conditions (type of gas and flow rate, output, process time, etc.) in an oxygen (O 2 ) atmosphere. Can be performed accordingly.
  • the process sequence of reactive ion etching loads the specimen, identifies the specimen loaded in the chamber, and then sets the set reactive ion etching environmental conditions (vacuum degree, type and amount of gas, etc.).
  • the reactive ion etching environmental conditions may form conditions in the chamber by flowing 50 sccm of oxygen gas (O 2 gas) at a predetermined vacuum degree (100 mtorr).
  • the plasma is floated at an output of 50 W and surface treated, and the specimen is recovered. From the surface treatment, the nanofiber surface is changed to hydrophilic, and the thickness (diameter) of the nanofiber is reduced.
  • the method for producing a hazardous substance collection filter according to an embodiment of the present invention may induce physical and chemical property changes of nanofibers by surface treatment of reactive ion etching on nanofibers.
  • the physical property change is that the thickness (diameter) of the nanofibers is reduced, and the thickness (diameter) of the nanofibers is reduced to ensure a smooth air flow to the filter.
  • the collection efficiency can be improved, and the specific surface area can be increased to extend the life of the filter.
  • the chemical property change is to increase the attraction and hydrophilicity with the target material, it is provided with the effect of improving the trapping ability (capturing force or adsorption force) of the target material.
  • the target material may refer to a harmful substance in the air such as fine dust, and is not limited to the concentration of fine dust, suspended dust (fine dust, PM10) or ultrafine dust (PM2.5).
  • Step 120 may be a step of surface treatment of the thermal processing (thermal annealing process) to the nanofibers to induce a change in the properties of the nanofibers.
  • the heat treatment process is performed under an inert atmosphere such as nitrogen and argon, and may be performed at a temperature of 275 ° C to 750 ° C.
  • the heat treatment process may be performed for 1 to 2 hours at a heating rate of 7 ° C / min to 20 ° C / min and 5 ° C / min to 20 ° C / min heat treatment under a pressure condition of the atmosphere.
  • the present invention is not limited thereto.
  • step 120 is a surface treatment of the nanofiber heat treatment process
  • the nanofiber may be significantly reduced in diameter and length than before heat treatment by the carbonization of the polymer after the heat treatment.
  • Step 120 may be a step of inducing a characteristic change of the nanofibers by surface treatment of a plasma coating for plasma vapor deposition of the mixed gas on the nanofibers.
  • the plasma coating may use any one or a mixture of carbon fluoride (CF 4 ), argon (Ar), xenon (Ze), helium (He), nitrogen (N 2 ), and oxygen (O 2 ). Plasma vapor deposition on the nanofibers.
  • CF 4 carbon fluoride
  • Ar argon
  • Ze xenon
  • He helium
  • N 2 nitrogen
  • O 2 oxygen
  • the surface-treated nanofibers of the plasma coating may activate the surface to induce chemical property changes, and the hydrophilicity may be improved by the oxygen plasma coating.
  • Step 120 may be a step of inducing a characteristic change of the nanofibers by surface treatment of a self-assembly monolayer (SAM) patterned on the nanofibers to form a plurality of lines.
  • SAM self-assembly monolayer
  • the surface treatment of the self-assembled monomolecular film is an organic monomolecular film formed spontaneously, for example, by using a spontaneous reaction of a silane with a surface having a hydroxy functional group to fix a portion bonded to the silane to the surface.
  • Step 120 may be a step of inducing a property change of the nanofibers by coating or replacing the surface of the nanofibers with conductive nanoparticles.
  • the surface treatment of nanofibers is intended to increase the chemical bonding strength with a target material according to physical and chemical property changes.
  • the surface treatment method using at least one of the above-described reactive ion etching, heat treatment process, plasma coating, self-assembled monolayer and conductive nanoparticles is preferably used in the market, but the physical process of the nanofibers And other processes or methods for changing chemical properties may be applied, but are not limited thereto.
  • the method for preparing a hazardous substance collection filter according to an embodiment of the present invention may include applying the surface treated nanofibers to the filter (step 130).
  • step 130 may be a step of coating and applying the surface-treated nanofibers to the filter support.
  • FIGS. 2A and 2B illustrate examples of nanofibers included in a hazardous substance collection filter according to an exemplary embodiment of the present invention.
  • Figure 2a shows an example of the surface treatment process for the nanofibers included in the harmful substance collection filter according to an embodiment of the present invention
  • Figure 2b shows a single nanofiber in the process performed in Figure 2a It is shown enlarged.
  • Hazardous substance trap filter 200 includes a nanofiber surface treated to increase the chemical bonding force between the target material and the nanofiber.
  • the nanofibers 210 in the harmful substance collection filter 200 are ultra-fine yarns having diameters of only tens to hundreds of nanometers (nm), compared to volume. Its large surface area can be used as a filter.
  • the material and type of the nanofibers are not limited.
  • the nanofibers 210 are surface treated (A) to increase the chemical bonding strength with the target material, and the harmful substance collecting filter 200 according to the embodiment of the present invention includes the nanofibers 220 treated with the surface.
  • the surface-treated nanofibers 220 may include reactive ion etching (RIE), a thermal annealing process, a plasma coating for plasma vapor deposition of a mixed gas, and a plurality of patterned nanofibers.
  • RIE reactive ion etching
  • the physical and chemical properties may be changed by surface treatment (A) of at least one of a self-assembly monolayer (SAM) forming a line, and coating or substitution of conductive nanoparticles.
  • SAM self-assembly monolayer
  • the harmful substance collection filter 200 by surface treatment (A) to the nanofibers 210, the physical and chemical properties of the surface-treated nanofibers 220 can be induced. .
  • the physical property change is to reduce the thickness (diameter) of the surface-treated nanofibers 220, the thickness (diameter) of the surface-treated nanofibers 220 is reduced to ensure a smooth air flow to the filter. Can be.
  • the collection efficiency can be improved, and the specific surface area can be increased to extend the life of the filter.
  • the chemical property change is to increase the attraction and hydrophilicity between the target material and the surface-treated nanofibers 220, it is provided with the effect of improving the trapping ability (capture or adsorption) of the target material.
  • the surface treatment method (A) using at least one of the above-described reactive ion etching, heat treatment process, plasma coating, self-assembled monolayer and conductive nanoparticles is preferably used in the market.
  • Other processes or methods for changing the physical and chemical properties of the nanofibers 220 may be applied, but are not limited thereto.
  • FIG. 3 is a graph showing the performance change of the surface-treated nanofibers according to the embodiment of the present invention.
  • FIG. 3 measures the change in performance for nanofibers without surface treatment (without RIE treatment), and changes in performance for 30s RIE treatment for surface treatment of reactive ion etching (RIE) for 30 seconds.
  • RIE reactive ion etching
  • the change in performance for the 60s RIE treatment of the surface treatment of the reactive ion etching (RIE) for 60 seconds was measured, and the nanofibers (90s RIE treatment) of the surface treatment of the reactive ion etching (RIE) for 90 seconds. The change in performance for was measured.
  • the x-axis (Operational time) of the graph represents time
  • the y-axis (Residual PM 2.5 concentration in chamber) represents the value of the fine dust (target material) residual concentration in the closed chamber.
  • the value of fine dust residual concentration in the closed chamber decreases with time of surface treatment of 0 seconds, 30 seconds, 60 seconds and 90 seconds, thereby improving the fine dust collection performance of the nanofibers. have.
  • the collection time of the fine dust is also shortened (collecting the fine dust faster and faster) according to the surface treatment time.
  • the method for manufacturing a hazardous substance collection filter according to an embodiment of the present invention may produce nanofibers having improved collection power in proportion to an increase in time of surface treatment of reactive ion etching (RIE).
  • RIE reactive ion etching
  • Figure 4 shows the image results for the characteristic change of the surface-treated nanofibers according to the embodiment of the present invention.
  • FIG. 4 shows image results for nanofibers whose physical and chemical properties are changed by surface treatment.
  • FIG. 4A is an image of nanofibers without surface treatment (without RIE treatment)
  • FIG. 4B is an image of 30s RIE treatment of surface treatment of reactive ion etching (RIE) for 30 seconds. It is.
  • FIG. 4C shows an image of a nanofiber (60s RIE treatment) surface-treated with reactive ion etching (RIE) for 60 seconds
  • FIG. 4D shows nano-surface treatment of reactive ion etching (RIE) for 90 seconds. Images of fibers (90s RIE treatment) were obtained.
  • the mean diameter of the unfinished nanofibers in FIG. 4A represents 449 ⁇ 43 nm
  • the average diameter of the surface treated nanofibers of reactive ion etching (RIE) for 30 seconds in FIG. 4B is 410 ⁇ 39 nm. Indicates.
  • the average diameter of the surface-treated nanofibers of reactive ion etching (RIE) for 60 seconds in FIG. 4C represents 347 ⁇ 43 nm
  • the surface-treated nanofibers of reactive ion etching (RIE) for 90 seconds in FIG. 4D represents 347 ⁇ 43 nm
  • the average diameter of 305 represents 305 ⁇ 37 nm.
  • the method for manufacturing a harmful substance collection filter according to an embodiment of the present invention may produce nanofibers whose diameter (thickness) decreases in proportion to an increase in time of surface treatment of reactive ion etching (RIE).
  • RIE reactive ion etching
  • FIG. 5 shows the results of surface modified XPS data of surface treated nanofibers according to an embodiment of the present invention.
  • FIG. 5A shows the results of surface modified X-ray Photoelectron Spectroscopy (XPS) data of unfinished nanofibers
  • FIG. 5B shows surface treated nanoparticles of reactive ion etching (RIE) for 30 seconds.
  • the results of the surface modified XPS data of the fibers are shown
  • FIG. 5C shows the results of the surface modified XPS data of the nanofibers surface treated with reactive ion etching (RIE) for 90 seconds.
  • XPS surface modified X-ray Photoelectron Spectroscopy
  • RIE reactive ion etching
  • FIG. 5C performed 3 cycles of 30 second surface treatment.
  • the x-axis (Binding energy) of the graph represents the binding energy
  • the y-axis (Intensity) represents the intensity
  • the graphs of the amide group (-CONH), ester group (-COOR) and carboxyl group (-COOH) formed on the nanofibers vary depending on the surface treatment time of 0, 30, and 90 seconds. You can check it. It can be seen from this that a chemical change of the surface-treated nanofibers of reactive ion etching (RIE) was induced.
  • RIE reactive ion etching
  • the manufacturing method of the harmful substance collection filter according to the embodiment of the present invention is a chemical change (increase in the chemical bonding force with the target material) and physical change (on the nanofiber surface with time of surface treatment of reactive ion etching (RIE) ( Reduced air pressure loss, longer life), thereby improving the performance of the filter.
  • RIE reactive ion etching
  • FIG 6 illustrates changes in contact angles of nanofibers before and after surface treatment according to an embodiment of the present invention.
  • FIG. 6A shows the contact angle for the nanofibers without surface treatment
  • FIG. 6B shows the contact angle for the nanofibers with surface treatment of reactive ion etching (RIE).
  • RIE reactive ion etching
  • the average contact angle with respect to water of the unfinished nanofibers in FIG. 6A represents 82 or more, and the average contact angle with respect to water of the surface treated nanofibers of reactive ion etching (RIE) in FIG. 6B shows less than 10.
  • RIE reactive ion etching
  • the nanofibers without surface treatment have higher hydrophobicity than the nanofibers with surface treatment of reactive ion etching (RIE).
  • RIE reactive ion etching
  • the method for manufacturing a hazardous substance collection filter according to an embodiment of the present invention can produce nanofibers having improved hydrophilicity by surface treatment of reactive ion etching (RIE), and the target material by nanofibers having improved hydrophilicity. Collection power can be improved.
  • RIE reactive ion etching
  • Figure 7 shows the performance change of the filter comprising a surface treated nanofiber according to an embodiment of the present invention.
  • FIG. 7 shows the surface of nanofibers (0 seconds) untreated, the surface of nanofibers (30s surface treated) with reactive ion etching (RIE) for 30 seconds, and the surface of reactive ion etching (RIE) for 60 seconds. Fine dust collection efficiency, pressure loss, reference value, contact value and performance index for the treated nanofibers (60s surface treatment) and the nanofibers treated with reactive ion etching (RIE) for 90 seconds.
  • the experimental results are shown in a table.
  • the contact angle is greatly reduced to an unmeasurable level (hydrophilicity) at 83 °, which is calculated from the QF value of the air filter, and is represented by 0.1264 to 30 seconds, 60 seconds and 90 seconds before surface treatment (0 seconds). It can be seen that it increases to 0.1564 with the time of the surface treatment of the second.
  • the method of manufacturing the hazardous material collection filter according to the embodiment of the present invention, as the time of surface treatment of reactive ion etching (RIE) increases, the fine dust collection efficiency increases, the pressure loss decreases, and the WHO reference value Nanofibers can be produced in which time to reach is reduced and figure of merit increases.
  • RIE reactive ion etching
  • the surface-treated nanofibers can be used to manufacture a filter having improved collection power by increasing the chemical bonding strength with the target material, and can be utilized as a more efficient air cleaning filter and application to an air cleaning device.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Filtering Materials (AREA)

Abstract

La présente invention concerne un filtre de collecte de substances nocives qui comprend une nanofibre traitée en surface, ce qui permet d'augmenter la force de liaison chimique entre une substance cible et la nanofibre et son procédé de fabrication, la puissance de collecte pouvant être améliorée par traitement de surface de la nanofibre pour changer des structures physiques et chimiques de la nanofibre, même sans utiliser de catalyseur.
PCT/KR2018/005075 2017-05-08 2018-05-02 Filtre de collecte de substances nocives hautes performances et son procédé de fabrication Ceased WO2018208040A2 (fr)

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KR1020170057365A KR101939991B1 (ko) 2017-05-08 2017-05-08 고성능의 유해물질 포집 필터 및 그의 제조 방법

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CN112717556A (zh) * 2020-11-30 2021-04-30 安徽元琛环保科技股份有限公司 一种具有脱硝脱二噁英功能的过滤材料的制备方法

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