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WO2018194431A2 - 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
WO2018194431A2
WO2018194431A2 PCT/KR2018/004648 KR2018004648W WO2018194431A2 WO 2018194431 A2 WO2018194431 A2 WO 2018194431A2 KR 2018004648 W KR2018004648 W KR 2018004648W WO 2018194431 A2 WO2018194431 A2 WO 2018194431A2
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WO
WIPO (PCT)
Prior art keywords
membrane
cnt
chitosan
layer
coating layer
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Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
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PCT/KR2018/004648
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English (en)
Korean (ko)
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WO2018194431A9 (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 comprising a metal substrate layer and a CNT / chitosan nano hybrid coating layer and an electrostatic precipitating system comprising the same.
  • Dust is classified into total dust, fine dust, and ultrafine dust according to its particle size.
  • the fine dust means that the diameter is 10 ⁇ m or less
  • the ultra-fine dust means that the diameter is 2.5 ⁇ m or less.
  • fine dust and ultrafine dust can penetrate into the alveoli of a person, which is a direct cause of various respiratory diseases after infiltration.
  • Such fine dust and ultrafine dust are composed of ionic 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, producing fine dust and ultra-fine dust. These materials are mainly generated from automobile exhaust or smoke from factories. Due to the harmfulness of these substances, countries around the world strictly regulate the concentration of fine dust and ultrafine dust.
  • the fine dust is generally about 1/10 of the thickness of the hair, while the ultra fine dust is very small, about 1/40 or less, so it is almost invisible to the human eye and can not be filtered out of the airways. do. This can lead to heart disease and respiratory diseases.
  • yellow dust from China occurs in spring, and in recent years, due to global warming, desertification of inland China has occurred, and the time of occurrence of yellow dust is also being accelerated.
  • Yellow dust from China was analyzed to be five times more toxic than domestic yellow dust.
  • the concentration of heavy metals is three times higher than that of Korea. Therefore, it is essential to wear a mask that can remove fine dust when going out.
  • fine dust caused by air pollution is also a major threat to health, attentive environment that should not have impurities such as operating room, intensive care unit and semiconductor process room, and underground spaces that are not well ventilated such as subway For example, it is very important to block fine dust and ultrafine dust even in office spaces where printers are frequently used. Therefore, the development of filters, such as for vehicles, masks, printers, air cleaners, air conditioners, electric cleaners, special clean rooms, etc. that can remove such fine dust or ultra-fine dust is becoming important.
  • Conventional anti-vibration filter uses a filter method using a woven fabric or a nonwoven fabric. In other words, a filter having pores smaller than the particle size was manufactured, and a method of filtering large particles was selected.
  • a conventional dust filter has two problems. First, there is a limit to removing nano-sized ultrafine particles whose particle size is smaller than 2.5 ⁇ m. Secondly, in order to effectively remove fine dust and ultrafine dust, the pores of the filter have to be made small, which makes it difficult to move the air. As a result, it is necessary to manufacture a dustproof filter that has pores of a suitable size, which allows free access of air and can effectively remove ultra fine dust.
  • the inventor of the present invention has completed the present invention by producing a membrane that has excellent electrical conductivity and can effectively collect fine dust even at a low current. Accordingly, the problem solving means of the present invention is as follows:
  • a membrane comprising a metal substrate layer and a CNT / chitosan nano hybrid coating layer coated on the metal substrate layer, wherein the CNT / chitosan nano hybrid is a CNT core surrounded by a chitosan shell.
  • the electrostatic dust collection system comprising the membrane of 1 above.
  • the membrane of the present invention includes CNTs in a high content, and has excellent electrical conductivity, and has excellent structural stability, and can effectively collect fine dust or ultrafine dust even at low current.
  • CNT / chitosan nano-hybrid by coating the CNT / chitosan nano-hybrid on the metal substrate it has sufficient electrical conductivity and can be mass-produced at high speed.
  • the membrane of the present invention is thus suitable for use in electrostatic precipitating systems.
  • FIG. 1 is a schematic of the core-shell structure of a CNT / chitosan membrane.
  • Figure 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 collection system of the present invention.
  • Figure 3 is a simplified diagram of the case where the membrane layer is disposed on one side of the filtration layer in the electrostatic dust collection system of the present invention.
  • FIG. 5 is an enlarged SEM image of FIG. 4C.
  • FIG. 8 shows a graph depicting the results of thermogravimetric analysis of pure CNT, chitosan and CNT / chitosan membranes.
  • FIG. 9A is a graph showing the change in thickness and surface resistance according to the CNT weight% change of the CNT / chitosan membrane
  • FIG. 9B is a graph showing the change in tensile strength and elastic modulus according to the CNT weight% change.
  • FIG. 10 is a graph showing the change in elongation rate according to the CNT weight% change of the CNT / chitosan membrane.
  • 11 is a graph showing tensile-stress curves of pure chitosan and CNT-chitosan 25, 50, 75, 85.
  • FIG. 13 shows XPS data C 1s (A), N 1s (B), and O 1s (C) of CNT / chitosan membranes.
  • FIG. 14 to 18 is a view showing the SEM image of the membrane surface of the present invention when exposed to outside air for 3 hours under a voltage of 0 to 12V, the case of 0V 14, 15V and 15V In FIG. 16 and 9V, FIG. 17 and 12V are shown in FIG. 18.
  • Figure 19 compares the membrane surface of the present invention after adsorption of fine dust and after washing it.
  • Example 20 is a photograph showing the Al / CNT membrane prepared in Example 2 of the present invention.
  • FIG. 21 shows a conceptual diagram and actual manufacturing results of the cylindrical electrostatic dust collecting system of the second embodiment of the present invention.
  • Example 22 is a graph showing the fine dust removal rate measured when only the nonwoven fabric is mounted in the cylindrical electrostatic dust collecting system of Example 2 of the present invention.
  • FIG. 23 is a graph showing the fine dust removal rate measured when only the nonwoven fabric and wool are mounted in the cylindrical electrostatic dust collecting system of Example 2 of the present invention.
  • Example 24 is a graph showing the fine dust removal rate measured when only the nonwoven fabric, wool and Al foil is mounted on the cylindrical electrostatic dust collecting system of Example 2 of the present invention.
  • Example 25 is a graph showing the fine dust removal rate measured in the cylindrical electrostatic dust collecting system of Example 2 of the present invention.
  • FIG. 26 is a measurement of the maximum adsorption capacity of the fine dust of the cylindrical electrostatic dust collecting system of Example 2 of the present invention, and an Al electrode and a carbon fiber electrode were used as a comparative example instead of the Al / CNT membrane.
  • Figure 27 shows the results of measuring the change in fine dust removal rate according to the size change of the cylindrical electrostatic filter, the left side when the size is 1.5 times (medium size in Example 2), the right side when the size is doubled ( The result of large size in Example 2 is shown.
  • the present invention includes a metal substrate layer and a CNT / chitosan nano hybrid coating layer coated on the metal substrate layer, wherein the CNT / chitosan nano hybrid is directed to a membrane wherein the CNT core is surrounded by a chitosan shell.
  • the CNT / chitosan nanohybrid has a core / shell structure and refers to a nanoparticle having a CNT core surrounded by a chitosan shell. If CNTs and chitosan are simply mixed or used in the form of composites, CNTs may not be uniformly distributed and may be concentrated in some areas, which may weaken the mechanical strength of the entire membrane and adversely affect the electrical conductivity of the membrane. Can be crazy On the other hand, the core / shell structure of the present invention allows the CNTs to be uniformly distributed, so that the membrane of the present invention can contain a high content of CNTs, while maintaining its excellent mechanical strength.
  • the core / shell structure of the CNT / chitosan nano hybrid of the present invention is shown in FIG. 1.
  • the CNT is short for carbon nanotubes, and includes both single-walled carbon nanotubes and multi-walled carbon nanotubes.
  • the chitosan refers to a polymer compound deacetylated chitin, the degree of deacetylation may be 75 to 85%, the molecular weight may be 50000 to 190000 Da, but within the range that can achieve the object of the present invention If not limited to this.
  • the metal substrate includes all metal substrates on which the CNT / chitosan nanohybrid can be coated, and is preferably a metal substrate having an oxide film formed on a surface thereof.
  • the surface of the metal substrate is oxidized, functional groups present in the oxidized portion of the surface and the chitosan of the CNT / chitosan nanohybrid can bond hydrogen, which allows 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 particularly preferably aluminum and copper.
  • the size of the manufacturable membrane can be increased, and the preparation 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 precipitating systems.
  • the coating layer preferably comprises 25 to 90% by weight of CNT based on the total weight of the coating layer. If the CNT content is less than this, the electrical conductivity of the membrane is low, which is not suitable for use in an electrostatic precipitating system, and if more than this, the mechanical strength of the membrane may be weakened.
  • the coating layer preferably has an electrical resistance of 50 ⁇ or less. If the electrical resistance is larger than this, a high voltage is required to generate an electric field, which lowers the energy efficiency of the electrostatic precipitating system.
  • the coating layer is preferably coated with a weight of 0.5 to 2.5 times the weight, based on the weight of the metal base layer, it is particularly preferably 1 to 1.5 times. If the weight of the coating layer is less than this, the dust collection capacity of the electrostatic dust collection system is lowered, if more than this may reduce the structural stability of the membrane.
  • the coating layer preferably has a specific surface area of 50 to 150m 2 / g. If the specific surface area is smaller than this, the dust collecting capacity of the electrostatic precipitating system will be reduced, and if the specific surface area is larger, the structural stability of the membrane may be reduced.
  • the present invention also the membrane layer; And a filtration layer.
  • the filtration layer refers to a layer having a function of filtering dust on a filtration principle, and may include a general cloth, a cabin filter, a nonwoven fabric or a wool layer.
  • the general fabrics collectively refer to woven and knitted fabrics composed of fibers.
  • the membrane layer may be disposed on either side or one side of the filtration layer.
  • the simplified electrostatic dust collection system when the membrane layer is disposed on both sides of the filtration layer is shown in FIG. 2, and the simplified electrostatic dust collection system when the membrane layer is disposed on one side of the filtration layer is simplified. Same as FIG. 3.
  • air containing dust is introduced parallel to the two membrane layers through the filtration layer. Due to the attraction by the electric field generated in the membrane layer by an external power source, the dust of the introduced air is attracted to both membrane layers and collected, and the dedusted air passes through the filtration layer and is discharged out of the dust collection system.
  • air containing dust is introduced in a direction perpendicular to the membrane layer through the filtration layer.
  • the dust from the introduced air is attracted to the membrane layer surrounding the filtration layer and collected by the attraction of the electric field generated in the membrane layer by an external power source, and the dedusted air passes through the filtration layer and is discharged outside the dust collection system. do.
  • the electrostatic dust collecting system of the present invention may have a planar shape or a cylindrical shape, and a representative example of the planar form is shown in FIG. 2, and a representative example of the cylindrical form is shown in FIG. 3.
  • any form can be used without limitation as long as it can utilize the principles of the electrostatic dust collecting system of the present invention.
  • the electrostatic dust collection system of the present invention has an electrical resistance of 50 ⁇ or less. If the electrical resistance is larger than this, a high voltage is required to generate the electric field required for driving the dust collecting system, thereby reducing the energy efficiency of the electrostatic dust collecting system.
  • the air velocity of the gas passing through the filtration layer is from 0.001 to 5 m / s. If the wind speed is lower than this, the amount of air that can be purified per unit time is not enough, if high, there is a problem that the dust collection performance is not enough.
  • 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, there is a problem that the dust collection efficiency is not sufficient.
  • Example 1 CNT / chitosan nano hybrid coating layer
  • Multi-walled carbon nanotubes > 95%, outer radius 20-30 nm, length 10-30 ⁇ m
  • EMP EM-Power Co., Republic of Korea
  • CNT carbon nanotubes
  • a membrane was prepared in the same manner as in Preparation Example 1, except that carbon nanotubes were used at 25 wt%.
  • the membranes were prepared in the same manner as in Preparation Example 1, except that 75% by weight of carbon nanotubes were used.
  • a membrane was prepared in the same manner as in Preparation Example 1, except that 85 wt% of the carbon nanotubes were used.
  • 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). . Samples were sputter-coated with gold prior to SEM analysis. The results are shown in Figures 4-6.
  • 4 is an HR-TEM (A), FE-SEM (B) image and 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 CNTs.
  • thermogravimetric analyzer Seiko Exstar 6000 TG / DTA6100, Japan
  • FTIR Fourier transform infrared spectrometer
  • Samples were heated in the range 25-900 ° C. at a rate of 10 ° C./min using 4 mg of sample.
  • FT-IR spectra were measured in the solid state and in the range from 400 to 4000 cm ⁇ 1 .
  • Experiments were also performed on pure chitosan and CNT for comparison, and the results of the FT-IR are shown in FIG. 7 and the results of TGA are shown in FIG. 8.
  • thermogravimetric analysis major mass loss occurred in the range of 600 to 700 ° C. for pure CNTs, but mass loss occurred in two steps for pure chitosan.
  • the first stage is near about 300 ° C. where the polymer structure is broken and the decomposition of glucosamine units occurs, and the second stage is 400 to 600 ° C. where oxidative degradation occurs.
  • the 50 wt% CNT-chitosan membrane showed a clear two stage degradation.
  • the first step is between 200 and 300 ° C. resulting from loss of chitosan, and the second step is between 500 and 600 ° C. where decomposition of CNT occurs.
  • the thermal decomposition temperature of both materials moved to the lower side as compared to the pure case. This is because the weight concentration of each component is half lower as compared to the pure case.
  • FIG. 9 shows a comparison of changes in thickness and resistance of chitosan and tensile strength and modulus of elasticity according to CNT content. Also shown in Figure 10 is a graph showing the change in elongation rate according to the CNT content.
  • Raman spectra are an efficient way to analyze carbon nanocomponents.
  • the D-band at 1350 cm ⁇ 1 shows the presence of sp3 hybrid carbon. It also relates to a disordered graphite structure proportional to the amount of amorphous carbon in the dispersed state.
  • the high frequency of 1580 cm -1 G-band shows the structural strength of sp2 hybrid carbon with CNT oscillation mode. The sharpness of the G and G ⁇ peaks is related to the fact that nanotubes may exhibit metal-like conductivity.
  • the C 1s, N 1s and O 1s of XPS data obtained from the functionalized CNTs exhibit binding energies of 280-295, 395-410 and 525-540eV, respectively.
  • the C 1s spectrum of the chitosan functionalized CNTs shows that the sp2 carbon atoms of the CNT molecules are strongly attached to the chitosan molecules.
  • These XPS data show that the CNT surface is well functionalized with chitosan.
  • the surface of the membrane when exposed to outside air for 3 hours under a voltage of 0 to 12V was observed by SEM image to qualitatively determine the degree of adsorption of fine dust.
  • FIG. 14 in the case of 3V, in FIG. 15, in the case of 6V, in FIG. 16, in the case of 9V, in FIG. 18, and in case of 12V, FIG. 18 is shown. It was. From this, it was confirmed that the surface of the membrane was covered with fine dust as the voltage increased and a strong electric field was generated.
  • Example 2 Membrane comprising metal layer and CNT / chitosan nano hybrid coating layer and electrostatic dust collection system using same
  • Chitosan was dissolved in 150 ml of 1% acetic acid and hydrochloric acid solution (pH 2.0), and CNT was added, followed by sufficient stirring.
  • Chitosan 0.7g and CNT 0.7g (Chit-pCNT50), Chitosan 0.35g and CNT 1.05g (Chit-pCNT75), Chitosan 0.14g and CNT 1.26g (Chit-pCNT90)
  • the solution was prepared and sufficiently dispersed through stirring and dispersing equipment. Then, the pH was slowly increased to 9-10 by adding 5% aqueous ammonia or basic solution to each solution.
  • a cylindrical electrostatic dust collecting system was manufactured.
  • a cylindrical frame was fabricated by 3D printing technique, and the dust collecting system was composed of a three-layer structure of a first filtration layer (nonwoven fabric), a second filtration layer (wool), and an electrostatic CNT filter layer, and a CNT-chitosan 50 on the CNT filter layer.
  • Al / CNT membrane using the membrane was applied.
  • the conceptual diagram and the actual production result thereof are shown in FIG. 21. Cylindrical frame is manufactured in three sizes: small, medium and large.
  • the small size is 10cm long, the outer diameter is 7cm, the inner diameter is 4cm, the medium size is 15cm, the outer diameter is 10.5cm, the inner diameter is 6cm, and the large size is 20cm. It has a diameter of 14 cm and an inner diameter of 8 cm.
  • a dust collecting system composed of only a nonwoven fabric or a nonwoven fabric / wool was used as a comparative example.
  • the removal rates for PM 1.0, 2.5 and 10 dusts were measured at constant wind speeds for the 2, 4, 6, 8 and 10 nonwoven fabrics.
  • 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. 22. It was confirmed that the nonwoven fabric alone did not remove PM 1.0 and 2.5 dusts well, and even if the number of nonwoven fabrics increased, only the removal rate for PM 10.0 dust increased, but the removal rates for PM 1.0 and 2.5 dust did not increase.

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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
KR20180118557A (ko) 2018-10-31
WO2018194432A2 (fr) 2018-10-25
WO2018194431A9 (fr) 2019-01-31
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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