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WO2018194431A9 - Membrane comprenant une couche de substrat métallique et une couche de revêtement nanohybride cnt/chitosane, et système de collecte de poussière électrostatique le comprenant - Google Patents

Membrane comprenant une couche de substrat métallique et une couche de revêtement nanohybride cnt/chitosane, et système de collecte de poussière électrostatique le comprenant Download PDF

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Publication number
WO2018194431A9
WO2018194431A9 PCT/KR2018/004648 KR2018004648W WO2018194431A9 WO 2018194431 A9 WO2018194431 A9 WO 2018194431A9 KR 2018004648 W KR2018004648 W KR 2018004648W WO 2018194431 A9 WO2018194431 A9 WO 2018194431A9
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WIPO (PCT)
Prior art keywords
membrane
cnt
chitosan
layer
electrostatic dust
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PCT/KR2018/004648
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English (en)
Korean (ko)
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WO2018194431A2 (fr
WO2018194431A3 (fr
Inventor
신원상
김한샘
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Industry Academic Cooperation Foundation of Dankook University
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Industry Academic Cooperation Foundation of Dankook University
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Publication of WO2018194431A3 publication Critical patent/WO2018194431A3/fr
Publication of WO2018194431A9 publication Critical patent/WO2018194431A9/fr
Anticipated expiration legal-status Critical
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    • 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
    • B01D46/0027—Filters or filtering processes specially modified for separating dispersed particles from gases or vapours with additional separating or treating functions
    • B01D46/0032—Filters or filtering processes specially modified for separating dispersed particles from gases or vapours with additional separating or treating functions using electrostatic forces to remove particles, e.g. electret filters
    • 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2239/00—Aspects relating to filtering material for liquid or gaseous fluids
    • B01D2239/02—Types of fibres, filaments or particles, self-supporting or supported materials
    • B01D2239/0216—Bicomponent or multicomponent fibres
    • B01D2239/0233—Island-in-sea
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2239/00—Aspects relating to filtering material for liquid or gaseous fluids
    • B01D2239/04—Additives and treatments of the filtering material
    • B01D2239/0435—Electret

Definitions

  • the present invention relates to a membrane including a metal base layer and a CNT / chitosan nanohybrid coating layer, and an electrostatic dust collecting system comprising the same.
  • Dust is classified into total dust, fine dust, and ultrafine dust depending on its particle size.
  • fine dust means a diameter of 10 ⁇ m or less
  • ultrafine dust means a diameter of 2.5 ⁇ m or less.
  • fine dust and ultrafine dust can penetrate into human alveoli, and it is a direct cause to cause various respiratory diseases after infiltration.
  • These fine dusts and ultrafine dusts are composed of ion components such as sulfate, nitrate, and ammonia, and harmful substances such as metal compounds and carbon compounds. These materials cause photochemical reactions in the atmosphere, resulting in fine dust and ultrafine dust, which are mainly generated from automobile exhaust gas or soot coming from factories. Due to the harmfulness of these substances, the concentration of fine dust and ultrafine dust is strictly regulated around the world.
  • Fine dust is generally about 1 / 10th of the thickness of hair, but ultrafine dust is very small, about 1/40 or less. It is hardly visible in human eyes and can not be filtered in airways. do. It causes heart disease and respiratory diseases.
  • Conventional dustproof filters use filter fabrics using woven fabrics or nonwoven fabrics. That is, a filter having pores smaller than the particle size was manufactured, and a method of filtering large particles was adopted.
  • these conventional dustproof filters have two problems. First, there is a limit to removing nano-sized ultrafine dust particles smaller than 2.5 mu m in size. Secondly, in order to effectively remove fine dust and ultrafine dust, the pores of the filter are inevitably reduced, which makes it difficult to move the air. As a result, it is necessary to fabricate a dust-proof filter which has pores of a proper size so that air can be freely flowed out and ultrafine dust can be effectively removed.
  • An object of the present invention is to provide a membrane and an electrostatic dust collecting system including the membrane, which have excellent electrical conductivity and can efficiently collect fine dust even at a low current.
  • the object of the present invention is as follows:
  • a membrane comprising a metal substrate layer and a CNT / chitosan nanohybrid coating layer coated on the metal substrate layer, wherein the CNT core is surrounded by a chitosan shell.
  • a capacitive dust collection system comprising the membrane of 1 above.
  • the membrane of the present invention contains CNT in a high content and has excellent electrical conductivity and is excellent in structural stability and can efficiently collect fine dust or ultrafine dust even at low current.
  • CNT / chitosan nanohybrid is coated on the metal substrate and it has sufficient electric conductivity and can be mass-produced at a high speed. Accordingly, the membrane of the present invention is suitable for use in an electrostatic dust collecting system.
  • Figure 1 is a schematic representation of the core-shell structure of a CNT / chitosan membrane.
  • Fig. 2 is a simplified view of the case where the membrane layer is disposed on both sides of the filtration layer in the electrostatic dust collecting system of the present invention.
  • FIG 3 is a simplified view of the case where the membrane layer is disposed on one side of the filtration layer in the electrostatic dust collecting system of the present invention.
  • Figure 7 shows the FTIR spectra of pure CNT, chitosan and CNT / chitosan membranes.
  • FIG. 9A is a graph showing changes in thickness and surface resistance according to the change in weight percentage of CNTs in a CNT / chitosan membrane
  • FIG. 9B is a graph showing changes in tensile strength and elastic modulus according to changes in weight percentage of CNTs.
  • FIG. 10 is a graph showing a change in elongation percentage according to a change in weight percentage of CNT of a CNT / chitosan membrane.
  • 11 is a graph showing the tensile-stress curves of pure chitosan and CNT-chitosan 25, 50, 75, 85.
  • FIG. 12 is a view showing a Raman spectrum of pure chitosan and CNT / chitosan membrane.
  • FIG. 13 is a diagram showing XPS data C 1s (A), N 1s (B), and O 1s (C) of a CNT / chitosan membrane.
  • FIG. 14 to 18 are graphs showing the results of observing the surface of the membrane of the present invention with an SEM image when exposed to the outside air for 3 hours under a voltage of 0 to 12 V.
  • the voltage is 0 V
  • FIG. 18 for 12V are graphs showing the results of observing the surface of the membrane of the present invention with an SEM image when exposed to the outside air for 3 hours under a voltage of 0 to 12 V.
  • Fig. 19 compares the membrane surface of the present invention after fine dust adsorption and after cleaning thereof.
  • Example 20 is a photograph showing the Al / CNT membrane prepared in Example 2 of the present invention.
  • FIG. 21 is a conceptual diagram and a production result of a cylindrical electrostatic dust collecting system according to the second embodiment of the present invention.
  • FIG. 22 is a graph showing a measured fine dust removal rate when only a nonwoven fabric is mounted on the cylindrical electrostatic dust collecting system of the second embodiment of the present invention.
  • FIG. 24 is a graph showing a measured fine dust removal rate when only a nonwoven fabric, wool, and Al foil are mounted on the cylindrical electrostatic dust collecting system of the second embodiment of the present invention.
  • 25 is a graph showing the dust removal rate measured by the cylindrical electrostatic dust collecting system of the second embodiment of the present invention.
  • Fig. 26 is a graph showing the maximum absorption capacity of fine dust in the cylindrical electrostatic dust collecting system of the second embodiment of the present invention.
  • an Al electrode and a carbon fiber electrode were used instead of an Al / CNT membrane.
  • FIG. 27 shows the measurement result of the change of the fine dust removal rate according to the size change of the cylindrical electrostatic filter.
  • the size is 1.5 times (medium size in the embodiment 2) and the size is twice the size on the right side (Large size in Example 2).
  • the present invention relates to a membrane comprising a metal substrate layer and a CNT / chitosan nanohybrid coating layer coated on the metal substrate layer, wherein the CNT core is surrounded by a chitosan shell.
  • the CNT / chitosan nanohybrid refers to a nanoparticle having a core / shell structure and a CNT core surrounded by a chitosan shell.
  • the CNTs may not be uniformly distributed and may be concentrated in some regions. This may result in a decrease in the mechanical strength of the entire membrane and an adverse effect on the electrical conductivity of the membrane I can go crazy.
  • the core / shell structure of the present invention allows CNTs to be uniformly distributed, so that the membrane of the present invention can contain a high content of CNTs while maintaining excellent mechanical strength.
  • the core / shell structure of the CNT / chitosan nanohybrid of the present invention is shown in Fig.
  • the CNT is an abbreviation of carbon nanotube and includes both single-walled carbon nanotubes and multi-walled carbon nanotubes.
  • the degree of deacetylation may be 75 to 85%, and the molecular weight may be 50000 to 190000 Da.
  • the chitosan But is not limited thereto.
  • the metal substrate includes a metal substrate on which the CNT / chitosan nanohybrid can be coated, and a metal substrate on which an oxide film is formed.
  • the oxidized portion of the surface and the functional groups present in the chitosan of the CNT / chitosan nanohybrid can make a hydrogen bond, which enables the substrate layer to be strongly bonded to the coating layer.
  • the metal of the metal base is preferably selected from the group consisting of iron, gold, silver, copper, platinum, titanium, aluminum and palladium, and is preferably aluminum-copper.
  • the size of the membrane that can be manufactured can be increased and the manufacturing time of the membrane can be shortened.
  • the metal substrate also imparts structural stability and electrical conductivity to the membrane, making the membrane of the present invention suitable for use in electrostatic dust collecting systems.
  • the coating layer preferably contains 25 to 90 wt% of CNT based on the total weight of the coating layer. If the content of CNT is smaller than this, the electrical conductivity of the membrane is deteriorated and it is not suitable to be used in the electrostatic dust collecting system, and if it is larger than this, the mechanical strength of the membrane may be weakened.
  • the coating layer has an electrical resistance of 50 ⁇ or less. If the electric resistance is larger than this, a high voltage is required to generate an electric field, which lowers the energy efficiency of the electrostatic dust collecting system.
  • the coating layer is preferably coated at a weight of 0.5 to 2.5 times the weight of the metal base layer, and particularly preferably 1 to 1.5 times. If the weight of the coating layer is less than that, the dust collecting ability of the electrostatic dust collecting system is lowered, and if it is larger than this, the structural stability of the membrane may be deteriorated.
  • the coating layer has a specific surface area of 50 to 150 m 2 / g. If the specific surface area is smaller than this, the dust collecting capacity of the electrostatic dust collecting system is lowered, and if it is larger than this, the structural stability of the membrane may be deteriorated.
  • the present invention also provides a membrane-electrode assembly comprising: the membrane layer; And a filtration layer.
  • the filter layer refers to a layer having a function of filtering dust by a filtering principle, and may include a general cloth, a cabin filter, a nonwoven fabric or a wool layer.
  • the above-mentioned general cloth generally refers to woven fabrics and knitted fabrics.
  • the membrane layer may be disposed on either or both sides of the filtration layer.
  • the simplification of the electrostatic dust collecting system in the case where the membrane layer is disposed on both sides of the filtration layer is shown in Fig. 2, and the electrostatic dust collecting system in the case where the membrane layer is disposed on one side of the filtration layer is simplified 3.
  • the electrostatic dust collecting system of the present invention may have a planar shape or a cylindrical shape.
  • a typical example of the planar shape is shown in FIG. 2, and a representative example of the cylindrical shape is shown in FIG.
  • any other form that can utilize the principle of the electrostatic dust collection system of the present invention is also possible without limitation.
  • the electrostatic dust collecting system of the present invention preferably has an electric resistance of 50 ⁇ or less.
  • the electric resistance is larger than this, a high voltage is required to generate an electric field necessary for driving the dust collection system, so that the energy efficiency of the electrostatic dust collection system is lowered.
  • the air velocity of the gas passing through the filtration layer is 0.001 to 5 m / s.
  • the amount of air that can be purified per unit time is not sufficient, and when the wind speed is higher, the dust collection performance is not sufficient.
  • the differential pressure before and after passing through the filtration layer is 100 Pa or less, and when the differential pressure is larger than this, the dust collection efficiency is not sufficient.
  • Example 1 CNT / chitosan nanohybrid coating layer
  • Multiwalled carbon nanotubes > 95%, outer radius of 20-30 nm, length of 10-30 ⁇ m
  • EMP EM-Power Co., Republic of Korea
  • CNTs carbon nanotubes
  • the dialyzed membrane was dialyzed against a dialysis membrane (Spectrum Laboratories, Worcester, GA) having a molecular weight of 12,000 to 14,000 and distilled water for 3 days, .
  • the CNT-chitosan solution was placed in a container of appropriate size, sonicated for 30 minutes, placed in a fume hood and room temperature for 2 days. The solution was then dried to produce a membrane.
  • a membrane was prepared in the same manner as in Production Example 1 except that the carbon nanotubes were used in an amount of 25 wt%.
  • a membrane was prepared in the same manner as in Production Example 1 except that the weight percentage of the carbon nanotubes was 75%.
  • a membrane was prepared in the same manner as in Production Example 1 except that the weight percentage of the carbon nanotubes was 85.
  • the shape of the CNT-chitosan membrane was analyzed using a high resolution electron transmission microscope (HR-TEM; JEM 3010, JEOL, Japan) and a field emission scanning electron microscope (FE-SEM; MIRA II LMH microscope, Tescan, Czech Republic) . Prior to SEM analysis, the samples were sputter-coated with gold. The results are shown in Figs. 4-6.
  • 4 is an HR-TEM (A), FE-SEM (B) image and a photograph (C) of CNT-chitosan 50.
  • 5 is an enlarged view of C of FIG. 4 by SEM.
  • 6 is an HR-TEM photograph of CNT-chitosan 25, 50, 75 and pure CNT.
  • thermogravimetric analyzer Seiko Exstar 6000 TG / DTA6100, Japan
  • FTIR Fourier transform infrared spectrometer
  • the sample was heated in the range of 25 to 900 DEG C at a rate of 10 DEG C / minute using a sample of 4 mg.
  • the FT-IR spectrum was measured in the solid state and in the range of 400 to 4000 cm <" 1 >.
  • experiments were also performed on pure chitosan and CNT, and the FT-IR results are shown in FIG. 7, and the TGA results are shown in FIG.
  • the first step is a step at about 300 DEG C where the polymer structure is broken and the decomposition of the glucosamine unit occurs
  • the second step is a step at 400 to 600 DEG C at which oxidative decomposition occurs.
  • a 50 wt% CNT-chitosan membrane showed a distinct two-step degradation.
  • the first step is a step of 200 to 300 ° C resulting from the loss of chitosan
  • the second step is a step of 500 to 600 ° C at which decomposition of CNT occurs.
  • the thermal decomposition temperature of the two materials was shifted to the lower side as compared with the pure case. This is because the weight concentration of each component is half as low as in the pure case.
  • FIG. 10 is a graph showing that the elongation percentage changes according to the CNT content.
  • Raman spectra are an efficient way to analyze carbon nanomaterials.
  • the D-band at 1350 cm -1 shows the presence of sp3 hybrid carbon. It is also related to disordered graphite structure proportional to the amount of amorphous carbon in the dispersed state.
  • the high-frequency 1580 cm -1 G-band shows the structural strength of the sp 2 hybrid carbon according to the vibration mode of the CNT. The sharpness of the G and G 'peaks is related to the ability of the nanotubes to exhibit metal-like conductivity.
  • C 1s, N 1s and O 1s of the XPS data obtained from the functionalized CNTs represent binding energies of 280-295, 395-410 and 525-540 eV, respectively.
  • the C 1s spectrum of chitosan functionalized CNTs shows that the sp2 carbon atoms of CNT molecules strongly attached to chitosan molecules are present in large amounts.
  • These XPS data show that the CNT surface is well functionalized with chitosan.
  • the surface of the membrane when exposed to the outside air for 3 hours under a voltage of 0 to 12 V was observed with an SEM image to qualitatively determine the degree of adsorption of the fine dust.
  • 19 in case of 0 V, 15 in case of 3 V, 16 in case of 6 V, 17 in case of 9 V, and 18 in case of 12 V, and the surface of the membrane after the fine dust adsorption and after washing thereof are compared Respectively. From this, it is confirmed that the surface of the membrane is covered with fine dust as the voltage increases and a strong electric field is generated.
  • Example 2 Membrane containing metal layer and CNT / chitosan nanohybrid coating layer and electrostatic dust collecting system using the same
  • Chitosan was dissolved in 150 ml of 1% acetic acid and hydrochloric acid solution (pH 2.0), CNT was added, and the mixture was stirred sufficiently.
  • the amount of chitosan and CNT was varied by 0.7g of chitosan, 0.7g of Chit-pCNT50, 0.35g of chitosan, 1.05g of Chit-pCNT75, 0.14g of chitosan and 1.26g of Chit-pCNT90.
  • the solution was prepared and sufficiently dispersed through a stirring and dispersing equipment. Then, 5% ammonia water or basic solution was added to each solution to slowly increase the pH to 9-10.
  • the Al thin film was flattened and spread on a hot plate, and the three solutions prepared above were separately dispersed on the thin film. Thereafter, the mixture was dried at a controlled temperature ranging from 60 to 70 ° C., immersed in 5% ammonia water for a while, taken out, washed with water and ethanol, and dried to prepare a membrane including an aluminum layer and a CNT / chitosan nanohybrid coating layer. Al / CNT membrane. In the case of the membrane not including the aluminum layer, it took 5 days to manufacture at the normal temperature condition, but it was possible to manufacture a large-sized membrane in one minute on the Al thin film. Its nano-surface area was measured to be at least 80 m 2 / g.
  • Fig. 20 is a photograph of the surface of the Al / CNT thus produced.
  • a cylindrical electrostatic dust collection system was fabricated to apply the membrane prepared in Production Example 2-1 to air cleaners and building ventilators.
  • a cylindrical frame was fabricated by 3D printing technique.
  • a dust collecting system was constructed with a three-layer structure consisting of a first filter layer (nonwoven fabric), a second filter layer (wool) and an electrostatic CNT filter layer.
  • CNT-chitosan 50 Al / CNT membrane using membrane was applied.
  • a conceptual diagram and a production result thereof are shown in Fig.
  • the cylindrical frame is made of three sizes, small size, medium size and large size. Small size is 10cm in length, 7cm in outer diameter, 4cm in inner diameter, 15cm in middle size, 10.5cm in outer diameter, 6cm in inner diameter, A diameter of 14 cm, and an inner diameter of 8 cm.
  • a nonwoven fabric or a nonwoven fabric / wool alone collecting system was used as a comparative example.
  • the PM 1.0, 2.5, and 10 dust removal rates were measured at constant wind speed.
  • the PM 1.0, 2.5, and 10 dusts refer to dusts having particle diameters of 1, 2.5, and 10 ⁇ m or less, respectively.
  • the results are shown in Fig. It was confirmed that the PM 1.0 and 2.5 dusts were not removed well by the nonwoven fabric alone, and the PM10.0 dust removal rate increased only when the nonwoven fabric longevity increased, and the PM 1.0 and 2.5 dust removal rates did not increase.
  • the removal rates of PM 1.0, 2.5 and 10 dusts were measured with 6 nonwoven fabrics as fixed values, and the amount of wool used was 2 g, 4 g, 6 g, 8 g, and 10 g at a constant wind speed. The results are shown in Fig. The removal rate of the nonwoven fabric was increased as a whole, but the removal rate was still about 50%. The PM 1.0 dust, which is the smallest dust, is removed only 34% even if the most wool is used Respectively.
  • the maximum adsorption capacity of fine dust was measured by setting 6 nonwoven fabrics and 10 g of wool as fixed values and mounting an Al / CNT membrane (CNT-chitosan 50) on the filter layer.
  • the Al / CNT membrane was replaced with an Al electrode and a carbon fiber electrode.
  • the experiment was carried out at 0.46V.
  • the results are shown in Fig.
  • the Al / CNT membrane retained 80% removal efficiency over 70 hours, while the remaining Al and carbon fibers retained their initial adsorption rates for 10 to 20 hours.
  • the maximum adsorption capacity of the fine dust of the Al / CNT membrane calculated from the above is 20.1 mg / g.

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

La présente invention concerne une membrane comprenant une couche de substrat métallique et une couche de revêtement nanohybride CNT/chitosane, et un système de collecte de poussière électrostatique le comprenant. La membrane selon la présente invention présente une excellente conductivité électrique et est ainsi capable de collecter efficacement la poussière, même avec un faible courant, et présente une excellente résistance mécanique et est ainsi appropriée pour une application dans divers types de systèmes de collecte de poussière électrostatique.
PCT/KR2018/004648 2017-04-21 2018-04-20 Membrane comprenant une couche de substrat métallique et une couche de revêtement nanohybride cnt/chitosane, et système de collecte de poussière électrostatique le comprenant Ceased WO2018194431A2 (fr)

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PCT/KR2018/004648 Ceased WO2018194431A2 (fr) 2017-04-21 2018-04-20 Membrane comprenant une couche de substrat métallique et une couche de revêtement nanohybride cnt/chitosane, et système de collecte de poussière électrostatique le comprenant

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KR102120735B1 (ko) 2020-06-09
WO2018194431A2 (fr) 2018-10-25
KR20180118557A (ko) 2018-10-31
WO2018194432A2 (fr) 2018-10-25
WO2018194432A3 (fr) 2018-12-20
KR102137416B1 (ko) 2020-07-24
KR20180118555A (ko) 2018-10-31
WO2018194431A3 (fr) 2018-12-20
WO2018194432A9 (fr) 2019-01-31
CN110799257A (zh) 2020-02-14

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