KR20150023960A - Nanofiber filter using Electro-Spinning and Meltblown and its manufacturing method - Google Patents

Nanofiber filter using Electro-Spinning and Meltblown and its manufacturing method Download PDF

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KR20150023960A
KR20150023960A KR20130091655A KR20130091655A KR20150023960A KR 20150023960 A KR20150023960 A KR 20150023960A KR 20130091655 A KR20130091655 A KR 20130091655A KR 20130091655 A KR20130091655 A KR 20130091655A KR 20150023960 A KR20150023960 A KR 20150023960A
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heat
electrospinning
filter
spinning
resistant polymer
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KR20130091655A
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Korean (ko)
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박종철
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(주)에프티이앤이
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Priority to KR20130091655A priority Critical patent/KR20150023960A/en
Priority to PCT/KR2014/001571 priority patent/WO2015016450A1/en
Priority to EP14831905.6A priority patent/EP3029191A4/en
Priority to US14/909,395 priority patent/US20160193555A1/en
Publication of KR20150023960A publication Critical patent/KR20150023960A/en

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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
    • B01D39/1607—Other self-supporting filtering material ; Other filtering material of organic material, e.g. synthetic fibres the material being fibrous
    • B01D39/1623—Other self-supporting filtering material ; Other filtering material of organic material, e.g. synthetic fibres the material being fibrous of synthetic origin
    • D—TEXTILES; PAPER
    • D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
    • D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
    • D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
    • D04H1/42—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties characterised by the use of certain kinds of fibres insofar as this use has no preponderant influence on the consolidation of the fleece
    • D04H1/425—Cellulose series
    • D—TEXTILES; PAPER
    • D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
    • D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
    • D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
    • D04H1/42—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties characterised by the use of certain kinds of fibres insofar as this use has no preponderant influence on the consolidation of the fleece
    • D04H1/4282—Addition polymers
    • D04H1/4291—Olefin series
    • D—TEXTILES; PAPER
    • D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
    • D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
    • D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
    • D04H1/42—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties characterised by the use of certain kinds of fibres insofar as this use has no preponderant influence on the consolidation of the fleece
    • D04H1/4326—Condensation or reaction polymers
    • D04H1/4334—Polyamides
    • D—TEXTILES; PAPER
    • D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
    • D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
    • D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
    • D04H1/42—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties characterised by the use of certain kinds of fibres insofar as this use has no preponderant influence on the consolidation of the fleece
    • D04H1/4326—Condensation or reaction polymers
    • D04H1/435—Polyesters
    • D—TEXTILES; PAPER
    • D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
    • D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
    • D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
    • D04H1/42—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties characterised by the use of certain kinds of fibres insofar as this use has no preponderant influence on the consolidation of the fleece
    • D04H1/4374—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties characterised by the use of certain kinds of fibres insofar as this use has no preponderant influence on the consolidation of the fleece using different kinds of webs, e.g. by layering webs
    • D—TEXTILES; PAPER
    • D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
    • D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
    • D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
    • D04H1/44—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties the fleeces or layers being consolidated by mechanical means, e.g. by rolling
    • D04H1/46—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties the fleeces or layers being consolidated by mechanical means, e.g. by rolling by needling or like operations to cause entanglement of fibres
    • D04H1/498—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties the fleeces or layers being consolidated by mechanical means, e.g. by rolling by needling or like operations to cause entanglement of fibres entanglement of layered webs
    • D—TEXTILES; PAPER
    • D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
    • D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
    • D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
    • D04H1/54—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties by welding together the fibres, e.g. by partially melting or dissolving
    • D04H1/56—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties by welding together the fibres, e.g. by partially melting or dissolving in association with fibre formation, e.g. immediately following extrusion of staple fibres
    • D04H1/565—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties by welding together the fibres, e.g. by partially melting or dissolving in association with fibre formation, e.g. immediately following extrusion of staple fibres by melt-blowing
    • D—TEXTILES; PAPER
    • D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
    • D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
    • D04H1/70—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres
    • D04H1/72—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres the fibres being randomly arranged
    • D04H1/728—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres the fibres being randomly arranged by electro-spinning
    • 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
    • B01D2239/0622—Melt-blown
    • 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

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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Mechanical Engineering (AREA)
  • Nonwoven Fabrics (AREA)
  • Spinning Methods And Devices For Manufacturing Artificial Fibers (AREA)

Abstract

The present invention relates to a heat-resistant multi-layer filter in which nanofibers are laminated by using melt-blown and electrospinning heat-resistant polymers on a cellulose substrate in order to improve the low heat resistance of existing filters. The multilayer heat-resistant filter thus manufactured is characterized by having heat-resistant polymers in a multilayer structure, so that not only the heat resistance is excellent but also the efficiency of the filter is excellent.

Description

TECHNICAL FIELD [0001] The present invention relates to a filter medium using melt blown and electrospinning,

The present invention relates to a multi-layered nanofiber filter having high heat resistance by continuously using melt blown and electrospinning and a method of manufacturing the same. More specifically, the present invention relates to a multi- And polyethylene terephthalate, electrospunning one of methaaramide, polyethersulfone and polyimide thereon and electrospinning the same to form a laminate of nanofibers, and a method for producing the same.

The air filter removes foreign substances such as dust and dust contained in the air when the combustion air sucked into the gas turbine is taken in the air and purifies the purified air to supply it to the gas turbine. Is weak at high temperature, and there is a problem that the foreign matter is not removed well.

In addition, most microfibers that are conventionally produced are prepared by spinning, such as melt spinning, dry spinning, wet spinning or the like, in which the polymer solution is forcedly extruded and spun through fine holes by mechanical force. However, the diameter of the nanofibers produced in this manner is in the range of about 5 to 500 mu m, and it is difficult to produce nanofibers of 1 mu m or less. Therefore, a filter composed of such a large-diameter fiber can filter contaminant particles having a large diameter, but it is practically impossible to filter nano-sized contaminant particles.

Generally, a gas turbine used in a thermal power plant sucks and compresses purified air from the outside, injects compressed air into the combustor together with the fuel, mixes the mixed air and fuel, And then injecting high-temperature and high-pressure combustion gas into the vanes of the turbine to obtain a rotational force.

Since these gas turbines are made up of very precise parts, they are subjected to periodic planned preventive maintenance and air filters are used for the pretreatment to purify the air in the compressor.

In order to solve the above problems, various methods for fabricating nano-sized fibers (nonwoven fabric) have been developed and used. Among them, a method for forming organic nanofibers includes forming nanostructured materials by block segments, Formation of nanofibers by polymerization using silica catalyst, nanofiber formation by carbonization process after melt spinning, nanofiber formation by electrospinning of polymer solution or melt, and the like.

When a nanofiber filter is fabricated using the nanofibers thus produced, the nanofiber filter has a larger specific surface area than the nanofiber filter having a larger diameter, has flexibility for surface functional groups, and has nano-sized pore size. It can be efficiently removed.

However, the implementation of the filter using the nanofibers is not easy to control the various conditions for the production because the production cost is low and the production of the filter using the nanofiber is not available at a low price. The present gas turbine, Filters used in furnaces and the like require heat resistance.

In general, a filter is a filtration device for filtering foreign matters in a fluid, and is divided into a liquid filter and an air filter. Among them, the air filter has been developed as a clean room where the biologically harmful substances such as particulate matter, germs and molds, bacteria and the like are completely removed from the air in order to prevent the deterioration of the high- Demand is gradually increasing as the usage area spreads day by day. Cleanroom applications are widely used in semiconductor manufacturing, computer equipment assembly, tape manufacturing, printing painting, hospitals, pharmaceutical manufacturing, food processing plants, agriculture, forestry and fisheries.

The air filter forms a porous layer of microporous structure on the surface of the filter media so that the dust does not penetrate into the filter media and performs filtration. However, the large particles are formed by the filter cake on the surface of the filter material, and the fine particles pass through the primary surface layer and gradually accumulate in the filter material, thereby blocking the pores of the filter. As a result, large particles and fine particles, which trap the pores of the filter, increase the pressure loss of the filter and deteriorate the life of the filter. In addition, conventional filter media have difficulties in filtering fine particles having a size of 1 μm or less .

On the other hand, the efficiency of the conventional air filter is measured by the principle that the static electricity is given to the fibrous aggregate constituting the filter filter material and the particles are collected by the electrostatic force. However, in recent years, EN779, the European air filter classification standard, has decided to exclude the filter efficiency due to the electrostatic effect in 2012, so that the actual efficiency of the conventional filter is lowered by more than 20% The use of glass fibers for environmental stability has been regulated in Europe and the United States due to the adverse effects of glass fiber used as a material for the environment.

In order to solve the above-mentioned problems, various methods of manufacturing nano-sized fibers and applying them to filters have been developed. When nanofibers are implemented in a filter, they have a large specific surface area compared to conventional filter media having a large diameter, good flexibility for surface functional groups, and nanoparticle pore size, so that harmful fine particles and gas can be efficiently removed It was.

However, since the production cost of the filter using the nanofibers is large, and it is difficult to control various conditions for production, etc., it is difficult to mass-produce the filter. Therefore, the filter using the nanofiber is produced at a relatively low cost I can not do that. Furthermore, filters used in gas turbines, blast furnaces and the like are demanding heat resistance.

The present invention relates to a heat-resistant polymer nanofiber comprising a first heat-resistant polymer nanofiber laminated on one side of a cellulose substrate by meltblown and a heat-resistant polymer nanofiber laminated by electrospinning a second heat-resistant polymer on one side of the first heat- Wherein the first heat-resistant polymer nanofiber includes one selected from the group consisting of polyamide, polyethylene, and polyethylene terephthalate, and the second heat-resistant polymer nanofiber includes at least one selected from the group consisting of meta-aramid, polyether Sulfone, and polyimide is used to produce a filter material having high heat resistance.

The present invention uses a heat-resistant polymer and is excellent in heat resistance. By using meltblown and electrospinning continuously, the process is efficient and cost-competitive as well as heat-resistant nanofibers and can be used as a high-efficiency filter .

1 is a schematic view of a filter manufactured by the present invention.
2 is a view showing an electrospinning apparatus used in the present invention.
3 is a block diagram of an electrospinning device used in the present invention.
4 is a view showing a nozzle block and a nozzle of an electrospinning apparatus used in the present invention.

Hereinafter, preferred embodiments of the present invention will be described in detail with reference to the accompanying drawings. The present invention is not limited to the scope of the present invention, but is merely an example, and various modifications can be made without departing from the technical spirit of the present invention.

The present invention relates to a method for producing a polymer electrolyte membrane, which comprises laminating a polymer selected from polyamide, polyethylene, and polyethylene terephthalate on a cellulose substrate with a meltblown on the cellulose substrate, and polymerizing a selected one of methaaramide, polyether sulfone, and polyimide And a step of laminating the nanofibers by electrospinning the polymer solution, and a method of manufacturing the nanofiber filter.

In the present invention, the base material is a cellulose base material having excellent heat resistance. Cellulose is produced by plant photosynthesis. Cellulose fibers such as cotton, hemp, and rayon are typical examples of cell membranes of higher plants. In the case of the surface first, it has a large specific gravity, and is a material which is relatively heat stable because of heat resistance and flame resistance. It has good hygroscopicity, strong acidity but strong alkali. Hygroscopicity and durability, and thus it is widely used as a wide range of coating materials, and many studies have been conducted to overcome the disadvantages through functional processing. Flax fiber is composed of 5-6 square, thick shell and small hollow fiber yarn. It has high strength and heat resistance and can be used stably at high temperature. In addition, there are cellulosic fibers such as ramie, hemp, and jute. The common feature is that it is made of a material with high heat resistance. It can be used as a heat-resistant filter base material that can operate stably at high temperatures.

In addition, the heat-resistant polymer resin used for electrospinning in the present invention is composed of a polymer having a melting point of 180 ° C or higher so that the nanofiber layer does not collapse due to melting even when the temperature is continuously increased. For example, the heat-resistant polymer resin constituting the heat-resistant polymer microfine fiber layer may be selected from the group consisting of polyamide, polyimide, polyamideimide, poly (meta-phenylene isophthalamide), polysulfone, polyetherketone, polyetherimide, , Aromatic polyesters such as polytrimethylene terephthalate and polyethylene naphthalate, polytetrafluoroethylene such as polytetrafluoroethylene, polydiphenoxaphospazene and polybis [2- (2-methoxyethoxy) phosphazene] Such as polyurethane copolymers including polyglycerol, polyglycerol, polyglycerol, polyglycerol, polyglycerol, polyglycerol, polyetherketone, polyglycerol, polyglycerol, polyglycerol, polyglycerol and polyetherurethane; cellulose acetate, cellulose acetate butyrate, cellulose acetate propionate and the like. A resin with no melting point refers to a resin that burns without experiencing a melting process even when the temperature rises above 180 ° C. The heat-resistant polymer resin used in the present invention is preferably soluble in an organic solvent for ultra-fine fiberization such as electrospinning.

Among the above-mentioned heat-resistant polymer resins, the most preferable heat-resistant polymer resin in the present invention is meta-aramid, polyether sulfone, and polyimide.

The meta-aramid is the first highly heat-resistant aramid fiber that can be used at 350 ° C for a short time and 210 ° C for continuous use. When exposed to temperatures above this temperature, it is carbonized without melting or burning like other fibers. Above all, unlike other products that are flame retarded or refractory treated, they do not emit toxic gases or harmful substances even when carbonized, and thus they have excellent properties as eco-friendly fibers.

In addition, the meta-aramid has a very strong molecular structure of the fiber itself, so it is not only strong in its original strength but also easily oriented in the fiber axis direction in the spinning stage to improve the crystallinity, .

 In general, the specific gravity of the meta-aramid is 1.3 to 1.4, and the weight average molecular weight is preferably 300,000 to 1,000,000. The most preferred weight average molecular weight is 300,000 to 500,000. Meta-aramids include meta-oriented aromatic polyamides. The polymer should have a fiber forming molecular weight, and may comprise a polyamide homopolymer, a copolymer and mixtures thereof, which are mainly aromatic.

 Wherein at least 85% of the amide (-CONH-) bonds are attached directly to the two aromatic rings. The ring may be unsubstituted or substituted. The polymer becomes a meta-aramid when the two rings or radicals are meta-oriented along the molecular chain with respect to each other. Preferably, the copolymer contains up to 10% other diamines substituted for the primary diamine used to form the polymer, or up to 10% other diacids substituted for the primary diacid chloride used to form the polymer It has a diacid chloride. Preferred meta-aramids are poly (meta-phenylene isophthalamide) (MPD-I) and copolymers thereof. One such meta-aramid fiber is < RTI ID = 0.0 > a < / RTI > children. Aramid fibers available from EI du Pont de Nemours and Company, but the meta-aramid fibers are available from Teijin Ltd., Tokyo, Japan. ≪ RTI ID = 0.0 > Possible trade names Tejinconex (R); NewStar TM meta-aramid available from Yantai Spandex Co. Ltd, Shandong, China; And Chinfunex (registered trademark) Aramid 1313, available from Guangdong Charming Chemical Co., Ltd., Shinshu, Guangdong, China.

The organic solvent is not particularly limited as long as it can sufficiently dissolve the polymer and is applicable to the charge induction spinning method. In addition, when the porous polymer nanofiber is produced by the charge-induced spinning method, since the organic solvent is almost removed, Anything that affects the characteristics may also be used. For example, propylene carbonate, butylene carbonate, 1,4-butyrolactone, diethyl carbonate, dimethyl carbonate, 1,2-dimethoxyethane, 1,3-dimethyl-2-imidazolidinone, N-dimethylformamide, N, N-dimethylacetamide, N-methyl-2-pyrrolidone, polyethylene sulfolane, tetraethylene glycol dimethyl ether, acetone, alcohol or mixtures thereof Can be selected and used.

Polyethersulfone (PES) is a transparent amorphous resin.

That is, since the polyether sulfone (PES) is amorphous, there is little deterioration of physical properties due to temperature rise, and the temperature dependence of the flexural modulus is very small, so that it hardly changes at 100 to 200 ° C. The load-strain temperature is 200 to 220 占 폚, and the glass transition temperature is 225 占 폚. In addition, the creep resistance up to 180 占 폚 is the most excellent among the thermoplastic resins, and has the characteristic of being resistant to hot water and steam at 150 to 160 占 폚. Therefore, due to the above characteristics of polyethersulfone, it is used for optical disks, magnetic disks, electric and electronic fields, hot water fields, automobile fields, heat resistant paints and the like.

Polyethersulfone has properties of improving heat resistance and thermal dimensional stability, and is not difficult to dissolve in a solvent. The molecular weight of the polyethersulfone is in the range of 8,000 to 200,000 in viscosity average molecular weight. When the viscosity average molecular weight is less than 8,000, the strength of the molded product is weak, which is easily undesirable. On the other hand, if it exceeds 200,000, the melt flowability tends to deteriorate, and it is difficult to obtain a good molded article. More preferably, the viscosity ranges from 400 to 1,200 cps. Examples of the solvent include dichloromethane, chloroform, tetorohydrofuran, methanol, ethanol, butanol, toluene, xylene, acetone, ethyl acetate, dimethylformamide, N-methyl-2-pyrrolidinone, dimethylacetamide But are not limited to these.

Polyimide is dissolved in a mixed solvent of tetrahydrofuran (THF) / dimethylacetamide (DMAc) (THF / DMAc) to prepare a spinning solution.

In the present invention, poly (amic acid) (PAA) was synthesized and dissolved in a THF / DMAc mixed solvent of tetrahydrofuran (THF) and dimethylacetamide (DMAc) to prepare polyamic acid , Polyimide nanofibers using electrospinning are prepared, and polyimide (PI) nanofibers can be prepared through imidization.

The polyimide is prepared by a two-step reaction.

In the first step, polyamic acid is prepared by adding dianhydride to a reaction solution in which diamine is dissolved. In order to increase the degree of polymerization, the reaction temperature, the water content of the solvent, And purity control. As the solvent used in this step, organic polar solvents such as dimethylacetamide (DMAc), dimethylformamide (DMF) and N-methyl-2-pyrrolidone (NMP) are mainly used. Examples of the anhydride include pyromellitic dianhydride (PMDA), benzophenonetetracarboxylic dianhydride (BTDA), 4,4'-oxydiphthalic anhydride (4,4'-oxydiphthalic anhydride) ODPA), biphenyltetracarboxylic dianhydride (BPDA), and bis (3,4'-dicarboxyphenyl) dimethylsilane dianhydride (SIDA). One can be used. Examples of the diamine include 4,4'-oxydianiline (ODA), p-penylene diamine (p-PDA) and o-penylenediamine o-PDA) may be used.

Figure pat00001

Reaction 1. Preparation of polyamic acid

The second step is the dehydration and ring-closing reaction step of producing polyimide from polyamic acid as the following four methods.

In the re-impregnation method, a polyamic acid solution is added to an excessive amount of a poor solvent to obtain a solid polyamic acid. As the re-precipitation solvent, water is mainly used, but toluene or ether is used as a co-solvent.

The chemical imidization method is a method in which a imidization reaction is chemically performed using a dehydration catalyst such as acetic anhydride / pyridine, and is useful for producing a polyimide film.

The thermal imidation method is a method in which the polyamic acid solution is heated to 150 to 200 ° C to thermally imidize the resin. In the simplest process or crystallization degree, the amine exchange reaction occurs when the amine type solvent is used, have.

In the isocyanate method, diisocyanate is used instead of diamine as a monomer, and when the monomer mixture is heated to a temperature of 120 ° C or higher, a polyimide is produced while CO 2 gas is generated.

Figure pat00002

Reaction formula 2. Preparation of polyimide

A meltblown and electrospinning device for preparing a heat-resistant polymer solution by dissolving the heat-resistant polymer in an organic solvent as described above, and continuously producing the nanofiber filter by meltblowing and electrospinning will be described as follows.

Meltblown is a method of spinning a synthetic polymer and producing microfine fibers as a uniform molten fiber by high pressure hot air. The polymer resin is a polyurethane (PU), a polyether urethane, a polyurethane copolymer, a cellulose acetate, a cellulose (PMMA), polymethyl acrylate (PMA), polyacrylic copolymer, polyvinyl acetate (PVAc), polyvinylacetate copolymer, polyvinyl alcohol (PVA) ), Polypropylene oxide (PP), polypropylene oxide (PP), polypropylene oxide copolymer, polycarbonate (PC), poly (ethylene terephthalate) Vinyl chloride (PVC), polycaprolactone (PCL), polyvinylpyrrolidone (PVP), polyvinylidene fluoride (PVdF) , Polyvinylidene fluoride copolymer, and polyamide.

In the present invention, the polymer is spun using a polymer selected from polyamide and polyethylene and polyterephthalate in meltblown.

In the present invention, the melt blown apparatus and the electrospinning apparatus are connected to collectors to continuously laminate the nanofibers.

2 is a schematic diagram of an electrospinning device.

As shown in the drawing, the electrospinning apparatus 10 of the present invention includes a spinning liquid main tank (not shown) in which a spinning liquid is filled and a weighing device for supplying a fixed amount of the polymer spinning solution filled in the spinning liquid main tank (3) in which a plurality of nozzles (2) in the form of a pin are arranged and a polymer spraying liquid in the spinning liquid main tank (1) is discharged from a nozzle A block 20 for accommodating therein a collector 4 spaced apart from the nozzle 2 in order to accumulate the usage liquid and a voltage generating device 1 for generating a voltage to the collector, And a case 8 made of a negative conductor.

In the present invention, one spinning liquid main tank (not shown) is provided. However, in the case where the spinning liquid is composed of two or more spinning liquids, two or more main spinning liquid main tanks may be provided, or one spinning liquid main tanks It is also possible to divide into two or more spaces and supply two or more polymer spinning solution filled in each divided space.

Meanwhile, in the present invention, the spinning solution supplied through the nozzle 2 of the nozzle block 3 in the block 20 is a polymer solution such as Meltblown.

Herein, in the present invention, the electrospinning device 10 uses a bottom-up electrospinning device for spraying the spinning liquid in the upward direction.

Meanwhile, in one embodiment of the present invention, a bottom-up electrospinning device for spraying the spinning solution upward by the electrospinning device may be used, but a top-down electrospinning device for spraying the spinning solution in the downward direction may be used. A composite electrospinning device in which a spinning device is used together may also be used.

With the above structure, the electrospinning apparatus 10 is configured such that the spinning liquid filled in the spinning liquid main tank in the block 20 continuously flows into the plurality of nozzles 2 to which a high voltage is applied through the metering pump And the spinning solution of the polymer supplied to the nozzle 2 is radiated and focused on the collector 13 having a high voltage through the nozzle 2 to form nanofibers (not shown) The fibers are laminated to produce a filter.

In the front end of the electrospinning device 10, there is provided a feed roller 11 for feeding a long sheet on which nanofibers are laminated by spraying a polymer spinning solution in each block 20, Up roller 12 for winding the sheet.

The long sheet is provided for preventing and transporting the nanofibers, and in the present invention, a base material 5 in which a heat-resistant polymer nanofiber is laminated on a cellulose base material in meltblown as a long sheet is used, The heat-resistant polymer spinning solution is layer-sprayed in the electrospinning device to form nanofibers.

Since the above-described electronic device and the electrospinning device are connected, more specifically, the meltblown nanofibers are laminated on the cellulose substrate and the electrospun nanofibers are laminated successively.

In an embodiment of the present invention, the cellulose base material 5 is used as a long sheet, but a release or nonwoven fabric may be used, but the present invention is not limited thereto.

That is, one side and the other side of the cellulose base 5 used as a long sheet in the present invention are wound around a feeding roller 11 provided at the front end of the electrospinning device 10 and a winding roller 12 provided at the rear end .

The feed roller 11 is connected to the meltblown device.

On the other hand, the electrospinning device of each block 20 is installed in the advancing direction (a) of the radiation with respect to the collector 4. Further, an auxiliary belt 6 is provided between each of the collectors 4 and the cellulose base material 5, and the cellulose fibers are stacked on the respective collectors 4 through the auxiliary belts 6 to form laminated nanofibers. (5) is transported in the horizontal direction. That is, the auxiliary belt 6 rotates in synchronization with the conveyance speed V of the cellulose base material, and has the auxiliary belt 7 for driving the auxiliary belt 6. The auxiliary belt roller 7 is an automatic roller having at least two frictional forces. Since the auxiliary belt 6 is provided between the collector and the cellulose base material 5, the cellulose base material 5 is smoothly conveyed without being attracted to the collector to which the high voltage is applied.

The spinning solution filled in the spinning liquid main tank in the block 20 of the electrospinning device 10 is discharged onto the surface of the cellulose base material 5 placed on the collector 4 through the nozzle 2 And the spinning liquid sprayed on the cellulose substrate 5 is accumulated to form the nanofibers. The auxiliary belt 6 is driven by the rotation of the auxiliary belt rollers 7 provided on both sides of the collector 4 to transfer the cellulose base material 5 to the block 20 at the rear end of the electrospinning device 10 ) So as to repeatedly perform the above-described process.

4, the nozzle block 3 includes a plurality of nozzles 2 arranged upward from the discharge port, a tube 43 formed by a row of nozzles 2, a spinning solution storage tank 44, And a spinning liquid circulating pipe (45).

First, the spinning liquid storage tank 44 connected to the spinning liquid main tank to receive and store the spinning solution is connected to the nozzle 2 through the spinning liquid circulating pipe 45 by the metering pump (not shown) And the spinning solution is supplied to the spinning solution. Here, the tube 43 having a plurality of nozzles 2 in a row is supplied with the same spinning solution from the spinning solution storage tank 44, but a plurality of spinning solution storage tanks are provided, It is also possible to supply a spinning liquid of different kinds to each of the tubes 43 and radiate them.

When radiated from the discharge port of the plurality of nozzles 2, the overflowed solution is moved to the overflow solution storage tank 41. The overflow solution storage tank 41 is connected to a spinning solution main tank (not shown) so that the overflow solution can be reused for spinning.

The main controller 30 of the present invention controls the spinning conditions in the course of the spinning and controls the amount of the spinning solution supplied to the nozzle block 3, 1 and controls the conveying speed V of each block according to the thickness of the nanofiber and the cellulose substrate measured by the thickness measuring device 9. [

The thickness measuring device 9 of the present invention is disposed opposite the cellulose base material 5 which is located at the front end and the rear end of the block 20 and in which nanofibers are laminated. The thickness measuring device 9 is connected to the main controller 30 for adjusting the radiation conditions of the electrospinning device 10 so that the thickness measuring device 9 measures the thickness of the nanofiber and the cellulose substrate 5 The main controller 30 controls the conveying speed V of each block 20 on the basis of one value. For example, if the thickness of the discharged nanofibers in each block 20 in the electrospinning is measured to be thinner, the feeding speed V of the block 20 located at the rear end is decreased, . Also, the main controller 30 increases the discharge amount of the nozzle block 3 and adjusts the intensity of the voltage of the voltage generator 1 to increase the discharge amount of the nanofibers per unit area, thereby uniformly controlling the thickness of the nanofibers It is possible.

The thickness measuring device 9 is provided with a thickness measuring unit consisting of a pair of ultrasonic longitudinal waves and a transverse wave measuring method for measuring the distance from the nanofiber on which the nanofibers are laminated to the cellulose base 5 by an ultrasonic measuring method , And the thickness of the nanofiber and the cellulose substrate 5 is calculated on the basis of the distance measured by the pair of ultrasonic measuring devices. More specifically, the ultrasonic longitudinal wave and the transverse wave are projected together on the cellulose base material 5 on which the nanofibers are laminated, and the time during which the ultrasonic signals of the longitudinal wave and the transverse wave move back and forth on the cellulose base material 5, From the predetermined calculation formula using the propagation time of the measured longitudinal waves and transverse waves and the temperature constant of propagation speed of longitudinal waves and transverse waves and the propagation speed at the reference temperature of the cellulose base material 5 in which the nanofibers are laminated, It is a thickness measuring device that calculates the thickness of a dead body.

The electrospinning device 10 used in the present invention is configured such that when the thickness deviation P of the nanofiber is less than a predetermined value, the feed velocity V is not changed from the initial value, , It is possible to control the feed speed V to be changed from the initial value, so that it becomes possible to simplify the control of the feed speed V by the feed speed V control device. Further, in addition to the control of the conveying speed V, the discharge amount of the nozzle block 3 and the intensity of the voltage can be adjusted. When the thickness deviation P is less than the predetermined value, the discharge amount of the nozzle block 3 and the intensity of the voltage It is possible to control the amount of discharge of the nozzle block 3 and the intensity of the voltage to be changed from the initial value when the deviation amount P is not less than the predetermined value without changing the initial value, It becomes possible to simplify control of the discharge amount and the intensity of the voltage.

In the present invention, the same polymer spinning solution is radiated in each block 20, but it is also possible to spin different kinds of polymer spinning solution for each block. In a block, two or more different polymer spinning solution It is also possible to radiate it. When at least two different kinds of spinning solutions are supplied and radiated for each block 20, it is possible that the polymer nanofibers of different kinds are successively laminated.

On the other hand, a laminating device 19 is provided at the rear end of the electrospinning device 10 of the present invention. The laminating device 19 applies heat and pressure to the cellulose base material on which the nanofibers are laminated, that is, the nanofiber filter is wound on the winding roller 12 to form nanofibers.

Hereinafter, one selected from the group consisting of polyamide, polyethylene and polyethylene terephthalate is melt-blended on the cellulose substrate by continuously using the meltblown apparatus and the electrospinning apparatus, and then, successively, a meta-aramid, A method of manufacturing a heat resistant filter for laminating nanofibers by electrospunning a polyimide heat resistant polymer will be described.

First, the heat-resistant polymer is dissolved in an organic solvent, the heat-resistant polymer solution is stored in a polymer solution reservoir of the meltblown apparatus, and the solution is supplied into a spinning nozzle through which the solution is discharged. The heat-resistant polymer solution supplied from the spinning nozzle is radiated by high-pressure hot air.

The spun meltblown fibers are transferred to the electrospinning device 10 to which they are connected.

The heat-resistant polymer is dissolved in an organic solvent and supplied to the spinning liquid main tank of the electrospinning device 10, and is continuously supplied in a constant amount into the nozzle 2 of the nozzle block 3 to which a high voltage is applied through a metering pump. The heat-resistant polymer solution supplied from each of the nozzles 2 is irradiated and focused on the collector 4 with a high voltage applied thereto through the nozzle 2, and the cellulose base material 5 ) To form a heat-resistant polymer nanofiber.

Here, in the electrospinning device 10, the cellulose base material on which the heat-resistant polymer nanofibers are laminated is composed of a feed roller 11 operated by driving of a motor (not shown), and an auxiliary belt 11 driven by the rotation of the feed roller 11, Is transferred to the block located at the rear end in the block located at the front end portion by the rotation of the first and second rollers 6, and the nonwoven fabric is formed while repeating the above-described process.

Here, the radiation voltage applied to the electrospinning device is preferably 1 kV or more, and preferably 15 kV or more.

DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS The present invention will now be described in more detail with reference to the following examples and drawings. It will be apparent, however, to those skilled in the art that the scope of the invention is not limited to the disclosed embodiments and modifications or improvements made therefrom.

[Example 1]

In the first section, meltblown melt spinning was carried out on the cellulose base material having a basis weight of 30 gsm under the conditions of a discharge amount of 7 kg / hr and a weight per unit area of 50 g / m < 2 > In a second section, a meta-aramid having a viscosity of 50,000 cps and a solid content of 20% by weight was dissolved in dimethylacetamide (DMAc), and the distance between the electrode and the collector was 40 cm, the applied voltage was 15 kV, the spinning liquid flow rate was 0.1 mL / A methacrylamide nanofiber is formed by electrospinning a meta-aramid solution to a thickness of 3 μm on a polyethylene fiber under conditions of 22 ° C. and a humidity of 20% to prepare a multi-layer filter material.

[Example 2]

In the first section, meltblown melt spinning was carried out on the cellulose base material having a basis weight of 30 gsm under the conditions of a discharge amount of 7 kg / hr and a weight per unit area of 50 g / m < 2 > (PAA) having a weight average molecular weight of 100,000 was dissolved in a mixed solvent (THF / DMAc) of tetrahydrofuran (THF) and dimethylacetamide (DMAc) The polyamic acid solution was electrospun to be 3 μm thick on the polyethylene fiber under the conditions of a distance of 40 cm from the electrode to the collector, an applied voltage of 15 kV, a spinning solution flow rate of 0.1 mL / h, a temperature of 22 ° C. and a humidity of 20% After formation of the fibers, the polyamic acid nanofibers are imidized with polyimide nanofibers by heating at 200 ° C to produce a multi-layer filter material.

[Example 3]

In the first section, meltblown melt spinning was carried out on the cellulose base material having a basis weight of 30 gsm under the conditions of a discharge amount of 7 kg / hr and a weight per unit area of 50 g / m < 2 > In a second section, polyethersulfone having a viscosity of 1,200 cps and a solid content of 20% by weight was dissolved in dimethylacetamide (DMAc), and the distance between the electrode and the collector was 40 cm, the applied voltage was 15 kV, the spinning solution flow rate was 0.1 mL / A polyethersulfone solution is electrospun to form a multilayer filter material on the polyethylene fibers under conditions of a temperature of 22 DEG C and a humidity of 20%.

[Comparative Example 1]

In the first section, a meta-aramid dope is prepared by dissolving meta-aramid having a viscosity of 50,000 cps and a solid content of 20% by weight in dimethylacetamide (DMAc). A 6 m-thick meta-aramid nanofiber was laminated on a cellulose substrate having a basis weight of 30 gsm under a condition of a distance between the electrode and the collector of 40 cm, an applied voltage of 15 kV, a spinning liquid flow rate of 0.1 ml / h, a temperature of 22 캜 and a humidity of 20% Thereby forming a filter medium.

- Heat resistance evaluation -

Examples 1 to 6 and Comparative Example 1 were heat-pressed under a linear pressure of 50 kg / cm at a temperature of 200 占 폚 to confirm the heat resistance.

- Filtration efficiency measurement -

The DOP test method was used to measure the efficiency of the fabricated nanofiber filter. The DOP test method measures the dioctyl phthalate (DOP) efficiency with an automated filter analyzer (AFT) of TSI 3160 from TSI Incorporated and measures the permeability, filter efficiency and differential pressure of the filter media material .

The automation analyzer is a device that automatically measures the velocity of air, DOP filtration efficiency, air permeability (permeability), etc. by passing DOP through the filter sheet by making particles of desired size and is a very important device for high efficiency filter.

The DOP filtration efficiency (%) is defined as:

DOP transmittance (%) = 1 - 100 (DOP concentration downstream / DOP concentration upstream)

Example 1 Example 2 Example 3 Comparative Example 1 Fiber Shrinkage (%) 3.3 3.2 3.3 5.0

Example 1 Example 2 Example 3 Comparative Example 1 0.35um DOP% 98 98 98 85

As described above, the multi-layered nanofiber filter manufactured by the embodiment of the present invention has higher heat shrinkage and filtration efficiency than the comparative example.

1, 1a, 1b: voltage generating device, 2: nozzle,
3: nozzle block, 4: collector,
5: base material, 6: auxiliary belt,
7: auxiliary belt roller, 8: case,
9: thickness measuring device, 10: electrospinning device,
11: feed roller, 12: take-up roller,
19: laminating apparatus, 20, 20a, 20b: block,
30: main control device, 41: overflow solution storage tank,
43: tube body, 44: spinning liquid storage tank,
45: circulating fluid pipe, 200: electrospun nanofiber,
300: meltblown nanofiber.

Claims (8)

A cellulose substrate;
A first heat-resistant polymer fiber laminated on one surface of the cellulose substrate by meltblown; And
A second heat-resistant polymer nanofibers laminated on one surface of the first heat-resistant polymer fiber by electrospinning a second heat-resistant polymer;
And a filter medium using electrospinning.
The method according to claim 1,
Wherein the first heat-resistant polymer comprises one polymer selected from the group consisting of polyamide, polyethylene, and polyethylene terephthalate, and a filter medium using electrospinning.
The method according to claim 1,
Wherein the second heat-resistant polymer nanofiber comprises one polymer selected from the group consisting of meta-aramid, polyethersulfone, and polyimide, and a filter medium using electrospinning.
Forming a first heat-resistant polymer fiber by spinning a first heat-resistant polymer on a cellulose substrate by meltblowing; And
Forming a second heat-resistant polymer nanofiber by spinning a spinning solution prepared by dissolving a second heat-resistant polymer on the first heat-resistant polymer fiber in an organic solvent;
And a method of manufacturing filter media using electrospinning.
5. The method of claim 4,
Wherein the first heat-resistant polymer is one selected from the group consisting of polyamide, polyethylene, and polyethylene terephthalate, and a method of manufacturing the filter medium using electrospinning.
5. The method of claim 4,
Wherein the second heat-resistant polymer nanofiber comprises one polymer selected from the group consisting of meta-aramid, polyethersulfone, and polyimide, and a method of manufacturing the filter medium using electrospinning.
5. The method of claim 4,
Wherein the meltblown and the electrospinning device are continuously connected to each other.
5. The method of claim 4,
Wherein the electrospinning uses a bottom-up electrospinning method.
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KR20130091655A KR20150023960A (en) 2013-08-01 2013-08-01 Nanofiber filter using Electro-Spinning and Meltblown and its manufacturing method
PCT/KR2014/001571 WO2015016450A1 (en) 2013-08-01 2014-02-26 Multi-layered nanofiber filter medium using electro-blowing, melt-blowing or electrospinning, and method for manufacturing same
EP14831905.6A EP3029191A4 (en) 2013-08-01 2014-02-26 Multi-layered nanofiber filter medium using electro-blowing, melt-blowing or electrospinning, and method for manufacturing same
US14/909,395 US20160193555A1 (en) 2013-08-01 2014-02-26 Multi-layered nanofiber medium using electro-blowing, melt-blowing or electrospinning, and method for manufacturing same

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2017028421A1 (en) * 2015-08-17 2017-02-23 博裕纤维科技（苏州）有限公司 Production equipment for nano-fiber deposit-based waterproof breathable fabric
KR20180083999A (en) * 2017-01-13 2018-07-24 주식회사 창명산업 Filtering media comprising porous network of heat resistant polymer fiber for dust collection of middle-high temperature exhaust gas, and preparation method thereof

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2017028421A1 (en) * 2015-08-17 2017-02-23 博裕纤维科技（苏州）有限公司 Production equipment for nano-fiber deposit-based waterproof breathable fabric
KR20180083999A (en) * 2017-01-13 2018-07-24 주식회사 창명산업 Filtering media comprising porous network of heat resistant polymer fiber for dust collection of middle-high temperature exhaust gas, and preparation method thereof

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