WO2020096249A1 - Filtre doté de fonctions super-hydrofuges et super-oléofuges, et appareil de fabrication associé - Google Patents

Filtre doté de fonctions super-hydrofuges et super-oléofuges, et appareil de fabrication associé Download PDF

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Publication number
WO2020096249A1
WO2020096249A1 PCT/KR2019/014251 KR2019014251W WO2020096249A1 WO 2020096249 A1 WO2020096249 A1 WO 2020096249A1 KR 2019014251 W KR2019014251 W KR 2019014251W WO 2020096249 A1 WO2020096249 A1 WO 2020096249A1
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Prior art keywords
ptfe
filter
repellent
foam coating
super
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PCT/KR2019/014251
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English (en)
Korean (ko)
Inventor
이명화
김한빈
김진식
이우진
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한국생산기술연구원
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Publication of WO2020096249A1 publication Critical patent/WO2020096249A1/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
    • B01D39/02—Loose filtering material, e.g. loose fibres
    • B01D39/06—Inorganic material, e.g. asbestos fibres, glass beads or fibres
    • 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
    • B01D2239/0471—Surface coating material
    • B01D2239/0492—Surface coating material on fibres
    • 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
    • B01D2239/06—Filter cloth, e.g. knitted, woven non-woven; self-supported material
    • B01D2239/0604—Arrangement of the fibres in the filtering material
    • B01D2239/0631—Electro-spun
    • 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
    • B01D2239/10—Filtering material manufacturing

Definitions

  • the present invention relates to a super-water-repellent, super-oil-repellent filter body and an apparatus for manufacturing the same.
  • Filter dust collectors are most commonly used to remove dust in the exhaust gas emitted from industrial combustion processes.
  • the filter dust collector used to remove fine dust exhibits very high dust collecting performance regardless of the type of dust or working conditions, and thus, most of the existing dust collectors are replaced by filter dust collectors.
  • the filter dust collector is a device for removing dust from the gas 11 by acting as a barrier when the filter gas (filtration bag) 10 passes through the filter gas 11.
  • the performance of the filter dust collector is influenced by the filter bag 10 mounted therein.
  • the dust in the exhaust gas is attached to and removed from the filter medium through mechanisms such as inertia impact, interception, and diffusion to the filter medium that acts as a barrier to the flow of fluid.
  • the type of filter bag used will vary depending on the temperature range of the exhaust gas. Polyester, Polypropylene filter bags at low temperatures below about 120 °C, NOMEX, PPS, P84, Laminated Membrane Filter in the range of 120 ⁇ 230 °C, At the above temperature, a metal filter ( ⁇ 500 ° C) and a ceramic filter ( ⁇ 1000 ° C) are used. In general, combustion takes place in the furnace and the temperature of the exhaust gas from the boiler is about 500 ° C, and when they go through the air preheater again, it becomes about 350 ° C. However, since the metal filter or the ceramic filter is too expensive, heat is exchanged again at 350 ° C. to drop the temperature to around 200 ° C., and then filtration is carried out.
  • the Laminated Membrane Filter can filter and collect at a relatively high temperature, but the temperature is 250 °C under the condition that a large amount of acidic and alkaline contaminants are present. If it becomes abnormal, the problem that the thin membrane layer disappears occurs.
  • a filter material that can be used at a temperature of 250 ° C. or more by foaming PTFE on a glass fiber fabric using a foam coating process has been developed (Registration No. 10-0934699).
  • the filter body Since the thickness of the PTFE layer is 100 ⁇ m, the filter body exhibits much better chemical and heat resistance compared to a laminated membrane filter having a membrane layer of 5 ⁇ m or less.
  • all of the above-mentioned filter bodies have a problem that is not very effective for removing highly sticky dust. That is, it is possible to collect high-adhesive dust with high efficiency, but it is difficult to dust with high efficiency.
  • the present invention is to develop a super-water-repellent, super-oil-repellent filter medium to effectively collect and recover highly sticky dust, and thereby to promote the use of a low-cost filter dust collector.
  • the first aspect of the present invention comprises a first step of foam coating and drying a foaming liquid for PTFE foam coating on a glass fiber filter to a constant thickness; A second step of electrospinning a solution containing PTFE and PVA on the surface of the grounded PTFE foam coating layer to volatilize the PVA fibers and attach only the PTFE fibers; A third step of attaching the PTFE powder sprayed by the electrostatic spraying method to the surface of the PTFE foam coating layer to which the PTFE fibers are attached; And a fourth step of curing the PTFE foam coating layer.
  • a second aspect of the present invention is a filter for removing adhesive dust in exhaust gas during fuel combustion, comprising: a glass fiber filter; Foam coating and drying PTFE foam coating layer with a constant thickness on the surface of the glass fiber filter PTFE foam coating; A PTFE fiber layer in which PTFE and PVA-containing solutions are electrospun on the surface of the PTFE foam coating layer to volatilize PVA fibers and adhere only PTFE fibers; And after forming a PTFE powder layer sprayed by the electrostatic spraying method on the surface of the PTFE foam coating layer is attached to the PTFE fiber, provides a filter medium characterized in that the PTFE foam coating layer is cured.
  • the third aspect of the present invention is a foam coater (Foam Coater) to form a PTFE foam coating layer by foam coating a foaming liquid for PTFE foam coating on a glass fiber filter surface to a constant thickness; Drying system for drying the PTFE foam coating layer formed in the foam coating machine (Drying system); A chamber that sequentially performs electrospinning and electrospraying while maintaining the temperature of PVA fiber volatilization, and electrospins the dried PTFE foam coating layer with a solution containing PTFE and PVA to volatilize the PVA fiber and then PTFE fiber A chamber for forming a PTFE fiber layer adhered only and forming a PTFE powder layer sprayed by an electrostatic spraying method on the surface of the PTFE foam coating layer to which the PTFE fibers are attached; And it provides a super water-repellent and super-oil repellent filter manufacturing apparatus, equipped with a curing system (Curing system) in the order of the process.
  • the fourth aspect of the present invention provides a high-precision dust removal filter dust collector having a filter bag made of the filter body of the second aspect.
  • the surface structure or pore size of the filter medium determines the dust layer in the initial stage of filtration, and the initial dust layer affects the formation of the subsequent dust layer and the filtration mechanism as filtration proceeds, so ultimately the first filtration Sieve structure is the dominant factor in dust filtration characteristics.
  • the pressure loss increases in proportion to the filtration speed, and a slight increase in the filtration speed in actual operation greatly affects the pressure loss and dust removal efficiency.
  • the pressure loss is the sum of the pressure loss of the filter medium itself and the pressure loss by the dust deposit layer, and the pressure loss of the filter medium itself is considerably lower than the pressure loss of the dust deposit layer.
  • the dust deposits act as a very good filter, but the pressure loss increases accordingly.
  • the viscosity and flow rate of the gas increase, which increases the pressure loss.
  • the clogging phenomenon of the filter medium is also caused by wet dust, and operation above the limit temperature rapidly degrades the filter medium.
  • Conditions for the filter medium to be provided are (i) sufficient mechanical strength against exhaustion, (ii) heat resistance depending on the properties of the treated gas, (iii) acid resistance, alkali resistance, and (iv) low hygroscopicity. , (v) Low pressure loss.
  • the super-water-repellent and super-oil-repellent filter bodies according to the present invention have excellent dedusting efficiency, and can be used as a filter for removing adhesive dust in industrial process exhaust gas,
  • the range of air permeability is 1 to 10 cm 3 / (cm 2 ⁇ s) at a pressure loss of 125 Pa, and the range of porosity may be 70 to 95%.
  • the air permeability is low, the pressure loss is high, but the dust collection efficiency is high, whereas when the air permeability is high, the pressure loss is low but the dust collection efficiency is low. Therefore, as the filter material of the filter dust collector is changed according to the demand of the customer, it is possible to select a filter medium that meets the demand.
  • a filter material having super water repellency and super oil repellency is essential.
  • the super water-repellent filter body may have a water contact angle of 150 ° or more.
  • the super-oil filter may have a contact angle of CH 2 I 2 of 120 ° or more.
  • the super-water-repellent and super-oil-repellent filter bodies may not form a dust layer on the filter body because the adhesive dust of the combustion exhaust gas, and help to effectively exhaust the adhesive dust of the combustion exhaust gas.
  • electrospinning PTFE fibers in the middle of the dryer 3 and the curing machine 6 of the PTFE foam coating system 4 And PTFE powder are equipped with an electrostatic spraying (5) system.
  • a foam coater that forms a PTFE foam coating layer by foam-coating a foaming liquid for PTFE foam coating on a surface of a glass fiber filter;
  • Drying system for drying the PTFE foam coating layer formed in the foam coating machine (Drying system);
  • a curing system is provided in the order of the process.
  • the super water-repellent and super-oil-repellent filter bodies of the present invention can be produced in the filter body manufacturing apparatus of the present invention.
  • the thickness of the glass fiber filter may be 400 to 1000 ⁇ m.
  • Polytetrafluoroethylene is a fluorine-based resin containing a fluorine compound represented by the following Chemical Formula 1, in which all of hydrogen in polyethylene is converted to fluorine.
  • PTFE is known under the trade name Teflon, and has chemical resistance, solvent resistance, dimensional stability, heat resistance, abrasion resistance, electrical insulation, and a smooth surface for almost all chemicals.
  • n is an integer between 100 and 10,000.
  • the “PTFE foam coating layer” may be a layer having an average pore size of 30 ⁇ m or less formed by foam coating on the glass fiber support with a coating solution containing PTFE resin, which is a heat-resistant resin.
  • the average pore size of the PTFE foam coating layer may be preferably 10 ⁇ m to 30 ⁇ m.
  • the “foaming liquid for PTFE foam coating” may be a coating liquid containing PTFE, a foam stabilizer, a foaming agent, and a thickener.
  • the foaming solution for PTFE foam coating is prepared by mixing PTFE, foam stabilizer, foaming agent and thickener in a weight ratio of 1: 0.05 to 0.1: 0.01 to 0.02: 0.01 to 0.05, preferably 1: 0.07: 0.02: 0.015 weight ratio. Can be.
  • the foaming solution for PTFE foam coating can use water as a solvent.
  • the foam stabilizer acts as a holding agent for the resin foam, and includes hydroxyethylcellulose, carboxymethylcellulose or ammonium stearate.
  • the blowing agent is a material that creates bubbles in the resin coating solution, and includes an anionic blowing agent containing sodium laurate and sodium stearate, or a nonionic blowing agent containing polyethylene glycol type and polyalcohol type.
  • the thickener acts to maintain the state in which the resin foam is attached to the fiber, and an acrylic thickener is preferred.
  • the foaming solution for PTFE foam coating may be first treated with a foam generator to form a foam solution, and then applied to the surface of the glass fiber support to form a foamed PTFE layer. Then, the support to which the foam solution is applied may be dried to form a dried foamed PTFE layer. Since the foam coating is a wet process, it is dried to evaporate by heating the water. During the drying process of the support to which the foam solution is applied, a stable microporous surface layer is formed. In the drying of the support to which the foam solution is applied, the primary drying may be performed at 80 ° C to 120 ° C, and the secondary drying may be performed at 180 ° C to 220 ° C.
  • the thickness of the PTFE foam coating layer may be preferably 5 ⁇ m to 100 ⁇ m.
  • Fiber membrane type PTFE has excellent flexibility and transmittance.
  • PTFE is difficult to process because of its unusually high melt viscosity and low solubility, making it difficult to manufacture PTFE nanofiber membranes.
  • Polyvinyl alcohol is a water-soluble polymer, which has excellent emulsion and adhesive properties, and does not mix with oil, lubricants, and organic solvents, but can stably disperse PTFE.
  • the filter body of the present invention is a PTFE fiber layer by electrospinning a solution containing PTFE and PVA on the surface of the PTFE foam coating layer to volatilize PVA fibers and attaching only PTFE fibers; And a PTFE powder layer sprayed by an electrostatic spraying method on the surface of the PTFE foam coating layer to which the PTFE fibers are attached.
  • PTFE and PVA Polyvinyl Alcohol
  • electrospinning an aqueous solution of PTFE and PVA (Polyvinyl Alcohol) is used, and in the chamber maintained at about 220 to 300 ° C, PVA fibers volatilize, leaving only PTFE fibers and adhering to the grounded fabric surface.
  • PTFE powder is electrostatically sprayed and attached to the PTFE fibers.
  • the weight ratio of PTFE and PVA is 2 to 5: 8 to 5, and only heat-treated PTFE fibers can be produced.
  • the average diameter of the manufactured PTFE fiber may be 0.1 ⁇ 2.5 ⁇ m.
  • PVA serves to increase the dispersibility of PTFE particles. Therefore, the PTFE concentration in the aqueous solution of PTFE used in the electrospinning method can be up to 60 wt%.
  • PTFE has a low surface free energy, and the fine PTFE fibers have a high specific surface area to prevent the penetration of water or oil components, so that water repellency and oil repellency can be enhanced by PTFE fibers attached to the surface of the PTFE foam coating layer. have.
  • the PTFE particles charged by the electrostatic spraying method can be attached to the surface of the PTFE foam coated filter in which the PTFE fibers are collected to form a PTFE powder layer.
  • the average particle diameter range of the attached PTFE powder may be 0.2 to 2.5 ⁇ m.
  • PTFE has a low surface free energy, and fine PTFE fibers have a high specific surface area to prevent water or oil from penetrating, and PTFE particles attached by electrostatic spraying method control surface roughness to enhance water and oil repellency. I can do it.
  • the PTFE foam coating layer is cured, it is a bond between the same PTFE components, so the PTFE foam coating layer, PTFE The bonding strength between the fiber layer and the PTFE powder layer is increased, and a surface layer having excellent surface strength can be formed.
  • the stable curing temperature may be 340 ⁇ 400 °C.
  • the bonding strength between the PTFE foam coating layer, the PTFE fiber layer, and the PTFE powder layer can be further increased through PTFE melt bonding, thereby increasing the strength of the microporous PTFE layer and smoothing its surface.
  • This compression treatment may be selectively performed, and is not an essential process.
  • the compression treatment may be preferably performed at a pressure of 200 psi to 700 psi.
  • the super water-repellent and super-oil-repellent filter bodies of the present invention have a structure of a porous web made of PTFE fibers, ultra-fine dust can also be collected through the structure of the porous web.
  • the pore size of a porous web made of PTFE fibers is determined by the thickness of the PTFE fiber layer and the diameter and filling rate of the strands of fibers in the PTFE web.
  • the average pore size of the PTFE fiber layer may be 2.5 ⁇ m or less, more preferably 0.1 ⁇ m to 2.5 ⁇ m.
  • the diameter of the PTFE fiber may be preferably 0.01 ⁇ m to 1 ⁇ m.
  • the removal efficiency of ultrafine dust is increased, and if the diameter of the PTFE fiber is larger than the upper limit, the dust collection efficiency is lowered.
  • the pressure loss is inversely proportional to the square of the fiber diameter.
  • the filter body according to the present invention is excellent in heat resistance and strong in heat shrinkage.
  • a method for producing super water-repellent and super-oil-repellent filter bodies according to one embodiment of the present invention is as follows.
  • a foaming solution for PTFE foam coating After mixing a PTFE resin, a foam stabilizer, a foaming agent, and a thickener, it is stirred at room temperature to prepare a foaming solution for PTFE foam coating.
  • the prepared foam for PTFE foam coating is introduced into the foam generator at a rate of 600 to 1350 g / min.
  • the foam generator quantitatively supplies air at a rate of 0.5 to 2 L / min to the foaming solution for PTFE foam coating
  • a foaming solution is generated by a stirrer rotating at a speed of 200 to 400 rpm.
  • the resulting foam liquid is supplied to the glass fiber filter by a coating liquid supply pump.
  • the glass fiber filter is transferred from the unwinder to the winder at a constant rate of 1.5 m / min to 2 m / min, while the foam coating is applied while the glass fiber filter is transferred from the unwinder to the winder. Is performed.
  • the foam liquid produced by the foam generator is supplied over the glass fiber filter through the coating liquid supply pipe by a coating liquid supply pump.
  • a knife-type blade (Knife coater) is installed on the conveyor belt, and the foamed liquid supplied over the glass fiber filter has a certain thickness, preferably about 0.3 mm to 1.0, by the blade while the glass fiber filter passes under the blade. It is adjusted to the thickness of mm.
  • the glass fiber filter coated with the foam is introduced into a dryer disposed at the rear end of the knife coater for drying of the foam solution applied on the surface. Then, a dried PTFE foam coated glass fiber filter is prepared, and then, an electrospinning module and an electrospraying module are introduced into a combined chamber. In a chamber maintained at PVA nanofiber volatilization temperature (220 ⁇ 300 °C), electrospinning the dried PTFE foam coating layer with a solution containing PTFE and PVA, volatilizes PVA fibers and forms a PTFE fiber layer with only PTFE fibers attached.
  • PVA nanofiber volatilization temperature 220 ⁇ 300 °C
  • the PTFE powder sprayed by the electrostatic spraying method is attached to the surface of the PTFE foam coating layer to which the PTFE fibers are attached.
  • the PTFE foam coating layer it is introduced into a curing machine disposed at the rear end.
  • the curing machine is maintained at a temperature of 340 ° C to 400 ° C for 1 minute to 20 minutes.
  • it is introduced into a compactor disposed at the rear end of the curing oven.
  • the pressure of the compactor compresses the coating layer to a pressure in the range of 200 psi to 700 psi, preferably 500 psi. Then, a glass fiber filter in which a coating layer of 0.1 mm to 0.2 mm is compressed, that is, a super water-repellent and super-oil-repellent filter body is prepared.
  • the filter body provided in the present invention exhibits super water repellency and super oil repellency, high adhesive dust in exhaust gas generated during combustion of various fuels using a low-cost filter dust collector equipped with the super water repellent and super oil repellent filter bags Can be removed with high efficiency.
  • FIG. 1 is a conceptual diagram showing a super water-repellent and super-oil-repellent filter manufacturing apparatus and manufacturing process according to an embodiment of the present invention.
  • FIG. 2 is a view of the surface of the GF / PTFE foam coated filter sintered at 350 ° C. for 10 minutes, magnified 400 times, and the contact angle measurement results showing the dust-off characteristics of the filter body.
  • FIG. 3 is an electrospinning of PTFE on a GF / PTFE foam coated filter sintered at 350 ° C for 10 minutes, and the surface of the filter sintered at the same temperature for 10 minutes is magnified 400 times with a microscope and the dusting characteristics of the filter body It is a result of measuring the contact angle.
  • Figure 4 shows the surface of the filter sintered for 10 minutes at the same temperature after electrostatic spraying PTFE to the filter sintered for 10 minutes at the same temperature after electrospinning PTFE on the GF / PTFE foam coated filter sintered at 350 ° C for 10 minutes. It is a drawing observed at a magnification of 400 times under a microscope and a contact angle measurement result showing the dust-off characteristics of the filter medium.
  • FIGS. 6 is a view showing a pressure loss change according to the surface filtration speed of the filter body of FIGS. 2 to 4;
  • FIG. 7 shows the measurement results of the filtration performance of the filter bodies of FIGS. 2 to 4.
  • the viscosity of the coating liquid foam is 10,000 cps, and the foaming ratio is 4 to 5: 1, and the shape of the surface layer is good.
  • the foam solution was applied to the glass fiber filter surface by a supply pump.
  • the surface of the glass fiber filter coated with the foam solution was adjusted to a thickness of 0.5 mm with a knife-shaped blade.
  • the feed pump speed was maintained at 30 rpm, and the feed speed of the glass fiber filter was maintained at 2 m / min.
  • the foam-coated glass fiber filter was put in a drying oven placed at the rear end of the blade and heat-treated for 5 minutes.
  • the heat treatment of the surface layer of the glass fiber filter coated with the foam solution was pre-heated at 80 ° C and post-heated at 220 ° C, and maintained for 5 minutes.
  • PTFE foam coating layer 60 wt% PTFE and 10 wt% PVA aqueous solution are electrospun on the dried PTFE foam coating layer surface to volatilize PVA fibers and form a PTFE fiber layer adhered only to PTFE fibers, followed by adhesion of PTFE fibers.
  • PTFE powder F104, Daikin, Japan
  • the filter cured the PTFE foam coating layer in a curing machine having an internal temperature of 350 ° C. for 10 minutes to complete the filter body.
  • foam coated PTFE webs and a PTFE fiber layer (fiber diameter: 1 ⁇ m) and a PTFE powder layer (powder particle size: 1 ⁇ m) formed thereon were formed on the surface of the filter body according to this embodiment.
  • Dust collection efficiency was calculated by measuring the number concentration of dust for testing with the Scanning Mobility Particle Sizer (SMPS, TSI Inc.) at the front and rear ends of the test filter, and the pressure loss affecting the performance of the filter was at the front and rear ends of the filter. Obtained by measuring the static pressure difference.
  • SMPS Scanning Mobility Particle Sizer
  • Figure 5 is a result of the measurement of the partial dust collection efficiency of the filter body of Figures 2 to 4, compared to the dust collection efficiency of the PTFE-coated filter on the glass fiber surface, dust collection of the filter is PTFE fiber electrospun on the surface It can be seen that the efficiency is increased, and the dust collection efficiency of the filter with PTFE powder attached to the surface is further increased. And, it can be seen that all filters show the lowest dust collection efficiency in the vicinity of the dust size of 0.1 ⁇ m.
  • Figure 6 shows the pressure loss change according to the surface filtration speed of the filter body of Figures 2 to 4, as opposed to the dust collection efficiency change, as shown in Figure 6, the pressure loss is PTFE coated on the surface of the glass fiber filtration It can be seen that while the sieve is the lowest, PTFE fibers are attached to the surface by electrospinning, and PTFE particles are attached by electrostatic spraying.
  • Equation 7 shows the measurement results of the filtration performance of the filter bodies of FIGS. 2 to 4, and it is difficult to evaluate the performance as a filter with dust collection efficiency and pressure loss, respectively. To compare this, the performance index of the filter defined by Equation 1 below is introduced.

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Geology (AREA)
  • Inorganic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Filtering Materials (AREA)
  • Filtering Of Dispersed Particles In Gases (AREA)

Abstract

La présente invention concerne un filtre doté de fonctions super-hydrofuges et super-oléofuges, et un appareil de fabrication associé. Le filtre est caractérisé par la formation : d'un filtre à fibres de verre ; d'une couche de revêtement en mousse de PTFE, obtenue au moyen de l'application, à une épaisseur prédéfinie, d'une solution moussante de revêtement en mousse de PTFE sur la surface du filtre à fibres de verre, et son séchage ; d'une couche de fibres de PTFE, obtenue par électrofilature d'une solution, contenant du PTFE et du PVA, sur la surface de la couche de revêtement en mousse de PTFE, afin de volatiliser une fibre de PVA, et de fixer uniquement une fibre de PTFE à ladite couche ; et d'une couche de poudre de PTFE obtenue par pulvérisation, par l'intermédiaire d'une pulvérisation électrostatique, de la surface de la couche de revêtement en mousse de PTFE comportant la fibre de PTFE fixée, puis le durcissement de la couche de revêtement en mousse de PTFE. Le filtre super-hydrofuge et super-oléofuge selon la présente invention présente une excellente efficacité de nettoyage de filtre, et peut ainsi être utilisé en tant que filtre permettant d'éliminer la poussière adhésive du gaz d'échappement d'un traitement industriel.
PCT/KR2019/014251 2018-11-07 2019-10-28 Filtre doté de fonctions super-hydrofuges et super-oléofuges, et appareil de fabrication associé WO2020096249A1 (fr)

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