KR101239136B1 - Method for Preparing Nano Fiber Web Comprising Apatite with High Antibacterial Function - Google Patents
Method for Preparing Nano Fiber Web Comprising Apatite with High Antibacterial Function Download PDFInfo
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- KR101239136B1 KR101239136B1 KR1020110014944A KR20110014944A KR101239136B1 KR 101239136 B1 KR101239136 B1 KR 101239136B1 KR 1020110014944 A KR1020110014944 A KR 1020110014944A KR 20110014944 A KR20110014944 A KR 20110014944A KR 101239136 B1 KR101239136 B1 KR 101239136B1
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- nanofiber web
- silver
- apatite
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- spinning solution
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- 239000002121 nanofiber Substances 0.000 title claims abstract description 56
- 229910052586 apatite Inorganic materials 0.000 title claims abstract description 34
- VSIIXMUUUJUKCM-UHFFFAOYSA-D pentacalcium;fluoride;triphosphate Chemical compound [F-].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O VSIIXMUUUJUKCM-UHFFFAOYSA-D 0.000 title claims abstract description 33
- 238000000034 method Methods 0.000 title claims description 16
- 230000000844 anti-bacterial effect Effects 0.000 title claims description 8
- 239000000243 solution Substances 0.000 claims abstract description 39
- 230000000845 anti-microbial effect Effects 0.000 claims abstract description 30
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 claims abstract description 24
- 229910052709 silver Inorganic materials 0.000 claims abstract description 22
- 239000004332 silver Substances 0.000 claims abstract description 22
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims abstract description 22
- 238000009987 spinning Methods 0.000 claims abstract description 22
- 229920000642 polymer Polymers 0.000 claims abstract description 16
- -1 silver ions Chemical class 0.000 claims abstract description 16
- 238000001523 electrospinning Methods 0.000 claims abstract description 13
- 239000006185 dispersion Substances 0.000 claims abstract description 11
- 238000004519 manufacturing process Methods 0.000 claims abstract description 11
- 229910001961 silver nitrate Inorganic materials 0.000 claims abstract description 11
- 239000007864 aqueous solution Substances 0.000 claims abstract description 8
- 229920002239 polyacrylonitrile Polymers 0.000 claims description 10
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 7
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 3
- 229920002635 polyurethane Polymers 0.000 claims description 3
- 239000004814 polyurethane Substances 0.000 claims description 3
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 3
- UKHWJBVVWVYFEY-UHFFFAOYSA-M silver;hydroxide Chemical compound [OH-].[Ag+] UKHWJBVVWVYFEY-UHFFFAOYSA-M 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 2
- 230000008014 freezing Effects 0.000 claims description 2
- 238000007710 freezing Methods 0.000 claims description 2
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 9
- 239000002245 particle Substances 0.000 description 5
- 241000894006 Bacteria Species 0.000 description 4
- 239000002904 solvent Substances 0.000 description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 239000000835 fiber Substances 0.000 description 3
- 239000000523 sample Substances 0.000 description 3
- 101710134784 Agnoprotein Proteins 0.000 description 2
- 241000588724 Escherichia coli Species 0.000 description 2
- 241000588747 Klebsiella pneumoniae Species 0.000 description 2
- 241000191967 Staphylococcus aureus Species 0.000 description 2
- 239000004599 antimicrobial Substances 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 239000013068 control sample Substances 0.000 description 2
- 239000012153 distilled water Substances 0.000 description 2
- 238000000724 energy-dispersive X-ray spectrum Methods 0.000 description 2
- 238000011534 incubation Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 2
- 229910052753 mercury Inorganic materials 0.000 description 2
- 244000005700 microbiome Species 0.000 description 2
- 108010023063 Bacto-peptone Proteins 0.000 description 1
- 229910014497 Ca10(PO4)6(OH)2 Inorganic materials 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- FOIXSVOLVBLSDH-UHFFFAOYSA-N Silver ion Chemical compound [Ag+] FOIXSVOLVBLSDH-UHFFFAOYSA-N 0.000 description 1
- 241000700605 Viruses Species 0.000 description 1
- 229910021536 Zeolite Inorganic materials 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 238000003915 air pollution Methods 0.000 description 1
- 150000001450 anions Chemical class 0.000 description 1
- 235000015278 beef Nutrition 0.000 description 1
- 210000000988 bone and bone Anatomy 0.000 description 1
- 230000001332 colony forming effect Effects 0.000 description 1
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 239000001963 growth medium Substances 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 229910052588 hydroxylapatite Inorganic materials 0.000 description 1
- 239000007943 implant Substances 0.000 description 1
- 238000011081 inoculation Methods 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 239000003456 ion exchange resin Substances 0.000 description 1
- 229920003303 ion-exchange polymer Polymers 0.000 description 1
- 238000010030 laminating Methods 0.000 description 1
- 239000002609 medium Substances 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 239000002923 metal particle Substances 0.000 description 1
- 235000015097 nutrients Nutrition 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000001012 protector Effects 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 239000000741 silica gel Substances 0.000 description 1
- 229910002027 silica gel Inorganic materials 0.000 description 1
- 150000003378 silver Chemical class 0.000 description 1
- 238000000527 sonication Methods 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000009210 therapy by ultrasound Methods 0.000 description 1
- 238000003911 water pollution Methods 0.000 description 1
- 239000010457 zeolite Substances 0.000 description 1
- 229910000166 zirconium phosphate Inorganic materials 0.000 description 1
- LEHFSLREWWMLPU-UHFFFAOYSA-B zirconium(4+);tetraphosphate Chemical compound [Zr+4].[Zr+4].[Zr+4].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O LEHFSLREWWMLPU-UHFFFAOYSA-B 0.000 description 1
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- 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
-
- A—HUMAN NECESSITIES
- A62—LIFE-SAVING; FIRE-FIGHTING
- A62B—DEVICES, APPARATUS OR METHODS FOR LIFE-SAVING
- A62B18/00—Breathing masks or helmets, e.g. affording protection against chemical agents or for use at high altitudes or incorporating a pump or compressor for reducing the inhalation effort
- A62B18/02—Masks
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/0007—Electro-spinning
- D01D5/0015—Electro-spinning characterised by the initial state of the material
- D01D5/003—Electro-spinning characterised by the initial state of the material the material being a polymer solution or dispersion
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
- D01F1/103—Agents inhibiting growth of microorganisms
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- 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
- D04H1/43—Acrylonitrile series
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- 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
- D04H1/4309—Polyvinyl alcohol
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- 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
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- D04H1/4326—Condensation or reaction polymers
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- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/32—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
- D06M11/36—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with oxides, hydroxides or mixed oxides; with salts derived from anions with an amphoteric element-oxygen bond
- D06M11/38—Oxides or hydroxides of elements of Groups 1 or 11 of the Periodic Table
- D06M11/42—Oxides or hydroxides of copper, silver or gold
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- 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
- B01D2239/0442—Antimicrobial, antibacterial, antifungal additives
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Abstract
본 발명은 항균성이 우수한 나노섬유 웹의 제조방법에 관한 것으로서, 은이온 담지용 아파타이트를 복합한 나노섬유 웹을 제조하고 은이온을 담지하여 항균성이 우수한 나노섬유 웹을 제조하는 방법에 관한 것이다.
본 발명은 수산화아파타이트를 분산시킨 분산용액에 고분자를 용해시켜서 방사용액을 제조하는 단계; 상기 방사용액을 전기방사하여 나노섬유 웹을 제조하는 단계; 상기 나노섬유 웹을 질산은 수용액에 침지하여 은이온을 흡착 및 담지시키는 단계를 포함하는 항균성이 우수한 은-나노섬유 웹의 제조방법을 제공한다.The present invention relates to a method for producing a nanofiber web excellent in antimicrobial activity, and to a method for producing a nanofiber web excellent in antimicrobial activity by preparing a nanofiber web comprising silver ions supported apatite and supporting silver ions.
The present invention comprises the steps of preparing a spinning solution by dissolving a polymer in a dispersion solution in which the apatite hydroxide is dispersed; Preparing a nanofiber web by electrospinning the spinning solution; It provides a method for producing a silver-nanofiber web excellent in antimicrobial comprising the step of immersing the nanofiber web in an aqueous solution of silver nitrate to adsorb and support silver ions.
Description
본 발명은 항균성이 우수한 나노섬유 웹의 제조방법에 관한 것으로서, 은이온 담지용 아파타이트를 복합한 나노섬유 웹을 제조하고 은이온을 담지하여 항균성이 우수한 나노섬유 웹을 제조하는 방법에 관한 것이다.The present invention relates to a method for producing a nanofiber web excellent in antimicrobial activity, and to a method for producing a nanofiber web excellent in antimicrobial activity by preparing a nanofiber web comprising silver ions supported apatite and supporting silver ions.
산업이 고도로 발전하면서 대기오염 및 수질 오염이 증가하여 심각한 환경문제가 대두 되고 있다. 따라서 대기나 수질에 존재하는 다양한 오염물질을 제거하기 위하여 공기정화기나 수처리 정수기 등이 많이 보급되고 있다. 공기정화기나 수처리 정수기에는 필터여재가 필수적으로 사용되고 있는데, 필터 여재에 공기중의 미생물이나 바이러스에 대해서 항균성을 부여하고 있다. 항균성 부여를 위한 항균제 물질들이 많이 공지되어 있는데, 예를 들어 제올라이트, 수산화아파타이트, 인산 지르코늄, 실리카 겔을 이용한 여러 계통의 무기 항균제가 알려져 있다. 이러한 무기계 항균제는 무기질 소재에 항균력이 우수한 금속이온을 치환시킨 것으로서, 3차원 구조를 가지고 있기 때문에 비표면적이 크고 내열성이 우수하다.Due to the high development of the industry, air pollution and water pollution have increased, causing serious environmental problems. Therefore, in order to remove various pollutants present in the air or water quality, air purifiers and water treatment water purifiers are widely used. Filter media are indispensably used in air purifiers and water treatment water purifiers. The filter media impart antimicrobial activity against microorganisms and viruses in the air. There are many known antimicrobial materials for imparting antimicrobial properties. For example, various types of inorganic antimicrobial agents using zeolite, apatite hydroxide, zirconium phosphate, and silica gel are known. Such an inorganic antimicrobial agent is a substitute for a metal ion having excellent antimicrobial activity in an inorganic material, and has a three-dimensional structure, and thus has a large specific surface area and excellent heat resistance.
항균성이 우수한 금속물질로서 수은과 은의 염류 및 그의 유기 화합물이 항균력이 강하다. 하지만 수은은 인체에 유해하기 때문에 향균성이 크면서 인체에는 무해한 은이 많이 이용되고 있다.As an excellent antimicrobial metal, mercury and silver salts and organic compounds thereof have strong antibacterial properties. However, mercury is harmful to the human body, which is highly antibacterial and harmless to the human body.
일반적으로 수산화아파타이트(Ca10(PO4)6(OH)2:HAp)는 생체 친화력 및 이온교환 능력이 우수하여 의학 및 치과의학 분야에서 인공 뼈 또는 인공치아와 같은 임플란트 소재로 사용되고 있고, 환경분야에서는 이온교환수지로서 중금속 제거를 위하여 사용되기도 한다.Generally, apatite hydroxide (Ca 10 (PO 4 ) 6 (OH) 2 : HAp) is used as an implant material such as artificial bones or teeth in the medical and dental fields because of its excellent biocompatibility and ion exchange ability. Is also used to remove heavy metals as ion exchange resins.
한국등록특허 제10-0536459호에서는 질산은을 함유하는 방사용액을 전기방사하여 은이 함유된 나노섬유 웹을 제조하는 방법을 제시하고 있다.Korean Patent Registration No. 10-0536459 proposes a method for producing a nanofiber web containing silver by electrospinning a spinning solution containing silver nitrate.
또한 한국등록특허 제10-0928232호에서는 은 입자를 방사용액에 분산시키고 이를 이용하여 나노섬유를 제조하는 방법을 제시하고 있다. 하지만, 상기 방법들은 은이온을 흡착하는 흡착제가 없어서, 은이온이 나노섬유 웹에 효과적으로 흡착되지 않는 문제점이 있고, 나노 은 금속입자가 고가이고, 분산시키기 어렵다는 문제점이 있다In addition, Korean Patent No. 10-0928232 proposes a method for preparing nanofibers by dispersing silver particles in a spinning solution. However, the methods do not have an adsorbent that adsorbs silver ions, there is a problem that the silver ions are not effectively adsorbed to the nanofiber web, there is a problem that the nano silver metal particles are expensive, difficult to disperse.
본 발명에서는 상기한 문제점을 해결하기 위하여 은 이온을 효과적으로 흡착하기 위하여 수산화아파타이트를 사용함으로써 항균성이 우수한 나노섬유 웹의 제조방법을 고안하였다. In the present invention, in order to solve the above problems, by using apatite hydroxide to effectively adsorb silver ions, a method for producing a nanofiber web excellent in antimicrobial properties was devised.
본 발명은 은 이온이 효과적으로 흡착되어 항균성이 우수한 나노섬유 웹을 제조하는 것을 목적으로 한다.An object of the present invention is to produce a nanofiber web with silver ions effectively adsorbed and excellent in antibacterial properties.
상기한 과제를 해결하기 위하여, 본 발명의 적절한 실시 형태에 따르면, 수산화 아파타이트 및 은을 포함하는 항균성이 우수한 나노섬유 웹의 제조방법을 제공한다.In order to solve the above problems, according to a preferred embodiment of the present invention, there is provided a method for producing a nanofiber web excellent in antimicrobial properties containing apatite hydroxide and silver.
본 발명의 다른 적절한 실시형태에 따르면, 수산화아파타이트를 분산시킨 분산용액에 고분자를 용해시켜서 방사용액을 제조하는 단계; 상기 방사용액을 전기방사하여 나노섬유 웹을 제조하는 단계; 및 상기 나노섬유 웹을 질산은 수용액에 침지하여 은이온을 흡착 및 담지시키는 단계를 포함하는 것을 특징으로 하는 항균성이 우수한 나노섬유 웹의 제조방법을 제공한다.According to another suitable embodiment of the present invention, the step of preparing a spinning solution by dissolving the polymer in a dispersion solution in which the apatite hydroxide is dispersed; Preparing a nanofiber web by electrospinning the spinning solution; And immersing the nanofiber web in an aqueous silver nitrate solution to adsorb and support silver ions.
본 발명의 또 다른 적절한 실시 형태에 따르면, 상기 수산화아파타이트는 방사용액 중량 대비 0.1 내지 5중량% 포함되어 있는 것을 특징으로 한다.According to another suitable embodiment of the present invention, the apatite hydroxide is characterized in that it contains 0.1 to 5% by weight relative to the weight of the spinning solution.
본 발명의 또 다른 적절한 실시 형태에 따르면, 질산은 수용액에 수산화아파타이트를 넣고 분산시키는 단계; 상기 분산액을 동결 및 건조하여 은-수산화아파타이트 복합체를 제조하는 단계; 상기 복합체를 고분자 용액에 첨가하여 방사용액을 제조하는 단계; 및 상기 방사용액을 전기방사하여 나노섬유 웹을 제조하는 단계를 포함하는 것을 특징으로 하는 항균성이 우수한 나노섬유 웹의 제조방법을 제공한다.According to another suitable embodiment of the present invention, the step of adding and dispersing apatite hydroxide in an aqueous solution of silver nitrate; Freezing and drying the dispersion to prepare a silver hydroxide apatite complex; Adding the complex to a polymer solution to prepare a spinning solution; And it provides a method for producing a nanofiber web excellent antibacterial comprising the step of producing a nanofiber web by electrospinning the spinning solution.
본 발명의 또 다른 적절한 실시 형태에 따르면, 상기 수산화아파타이트는 프로브형 초음파 분산기를 사용하여 20~40분간 분산시킨 것을 특징으로 한다.According to another preferred embodiment of the present invention, the apatite hydroxide is dispersed for 20 to 40 minutes using a probe-type ultrasonic disperser.
본 발명의 또 다른 적절한 실시 형태에 따르면, 상기 고분자는 폴리아크릴로니트릴, 폴리비닐알코올 및 폴리우레탄으로 이루어진 군에서 선택된 1종인 것을 특징으로 한다.According to another suitable embodiment of the present invention, the polymer is characterized in that the one selected from the group consisting of polyacrylonitrile, polyvinyl alcohol and polyurethane.
본 발명에서 제조된 나노섬유 웹은 은이온이 잘 흡착되어 있기 때문에, 항균성이 우수하다. 본 발명에 제조된 나노섬유 웹은 수처리 정수기 또는 공기 정화기의 필터 여재에 적용할 수 있고, 마스크, 상처보호대, 스캐 폴드나 항균성 라미네이팅용 멤브레인 필름에 사용할 수 있다.The nanofiber web prepared in the present invention has excellent antibacterial property because silver ions are well adsorbed. The nanofiber web prepared in the present invention can be applied to filter media of water treatment water purifiers or air purifiers, and can be used for membrane films for masks, wound protectors, scaffolds or antimicrobial laminating.
도 1은 본 발명에서 제조된 나노섬유 웹의 SEM 사진이다.
도 2는 본 발명에서 제조된 나노섬유 웹의 EDS 스펙트럼을 도시한 것이다.1 is a SEM photograph of the nanofiber web prepared in the present invention.
Figure 2 shows the EDS spectrum of the nanofiber web prepared in the present invention.
본 발명에서 은-나노섬유웹은 수산화아파타이트를 분산시킨 분산용액에 고분자를 용해시켜서 방사용액을 제조하는 단계; 상기 방사용액을 전기방사하여 나노섬유 웹을 제조하는 단계; 상기 나노섬유 웹을 질산은 수용액에 침지하여 은이온을 흡착 및 담지시키는 단계를 포함하는 방법으로 제조된다. In the present invention, the silver-nanofiber web is prepared by dissolving a polymer in a dispersion solution in which the apatite hydroxide is dispersed; Preparing a nanofiber web by electrospinning the spinning solution; The nanofiber web is prepared by a method comprising immersing and supporting silver ions by immersing in an aqueous solution of silver nitrate.
상기에서 수산화아파타이트 분산용액은 용매에 수산화아파타이트를 분산시켜서 제조한다. 상기 용매는 디메틸포름아미드(DMF), 메탄올, 증류수 등을 바람직하게 사용할 수 있으며, 고분자의 종류에 따라서 용매를 변경할 수 있다.The apatite hydroxide dispersion solution is prepared by dispersing apatite hydroxide in a solvent. The solvent may be preferably used dimethylformamide (DMF), methanol, distilled water and the like, the solvent can be changed according to the type of polymer.
수산화아파타이트는 방사용액 중량을 기준으로 0.1 내지 5중량%가 되도록 용매에 첨가하고, 프로브타입의 초음파 분산기(sonicator)로 20~40분간 분산시키는 것이 바람직하다. 본 발명에서는 초음파 분산기를 이용하여 수산화아파타이트의 입자크기가 1㎛이하가 되도록 조절하는 것이 바람직하다. 입자 크기가 1㎛ 이하인 경우 은이온 담지 능력 및 항균성이 우수해진다. Apatite hydroxide is added to the solvent so as to be 0.1 to 5% by weight based on the weight of the spinning solution, it is preferable to disperse for 20 to 40 minutes with a probe-type ultrasonic sonicator (sonicator). In the present invention, it is preferable to adjust the particle size of the apatite hydroxide to 1 μm or less using an ultrasonic disperser. When the particle size is 1 μm or less, the silver ion supporting ability and the antibacterial property are excellent.
다음으로 상기 아파타이트 분산용액에 고분자를 용해시키고 균일하게 분산켜서 방사용액을 제조한다. 상기에서 고분자는 전기방사가 가능한 고분자를 사용할 수 있는데, 구체적으로는 폴리아크릴로니트릴(PAN), 폴리우레탄, 폴리비닐알코올을 바람직하게 사용할 수 있다.
Next, the polymer is dissolved in the apatite dispersion solution and uniformly dispersed to prepare a spinning solution. The polymer may be a polymer capable of electrospinning, specifically, polyacrylonitrile (PAN), polyurethane, polyvinyl alcohol may be preferably used.
상기 고분자는 방사용액 총 중량 대비 5 내지 30중량%인 것이 바람직하다. 방사용액의 고분자 농도가 5중량%보다 낮으면 용액점도가 낮아서 나노섬유가 형성되지 않고 나노 스프레이 형태로 분말이 얻어지며, 농도가 30중량%를 초과하는 경우 용액점도가 너무 높아 전기방사가 불가하게 된다. The polymer is preferably 5 to 30% by weight based on the total weight of the spinning solution. If the polymer concentration of the spinning solution is lower than 5% by weight, the solution viscosity is low so that nanofibers are not formed and powder is obtained in the form of nano spray.If the concentration is higher than 30% by weight, the solution viscosity is too high to prevent electrospinning. do.
상기 방사용액은 전기방사법을 이용하여 섬유직경이 0.5 내지 1㎛인 나노섬유 웹으로 제조한다. 전기방사법은 공지의 방법을 사용할 수 있다.The spinning solution is prepared using a nanofiber web having a fiber diameter of 0.5 to 1 μm using an electrospinning method. The electrospinning method can use a well-known method.
제조된 나노섬유 웹은 50~200ppm의 질산은(AgNO3) 수용액에 5 내지 30분간 침지하여 은이온을 흡착 및 담지시킨다. 아파타이트를 포함하는 나노섬유 웹을 질산은 수용액에 침지함으로써, 은 이온이 웹의 표면에 흡착되게 되는데, 이 경우 항균능력이 섬유의 표면에만 부여되어 은 소모량을 최소화할 수 있고, 표면 항균처리로 항균특성이 우수하게 된다.The prepared nanofiber web is immersed in 50-200 ppm silver nitrate (AgNO 3 ) aqueous solution for 5-30 minutes to adsorb and support silver ions. By immersing the nanofiber web containing apatite in the silver nitrate aqueous solution, silver ions are adsorbed on the surface of the web. In this case, antimicrobial ability is given only to the surface of the fiber to minimize the consumption of silver. This will be excellent.
본 발명의 다른 적절한 실시 형태로서, 은-수산화아파타이트 복합체를 제조하고, 이를 고분자 용액에 복합하여 나노섬유 웹을 제조할 수 있다. In another suitable embodiment of the present invention, a silver-hydroxyapatite composite may be prepared and combined with a polymer solution to prepare a nanofiber web.
구체적으로는, 질산은 수용액에 수산화아파타이트를 넣고 프로브형 초음파 분산기를 시용하여 20~40분간 초음파 처리를 한다. 초음파 처리가 완료되면, 상기 용액을 여과하고 동결 건조하여 은-수산화아파타이트 복합입자를 제조한다. 제조된 은-수산화아파타이트 입자는 고분자가 용해된 방사용액에 1 내지 5중량%로 분산시키고, 공지의 전기방사법을 이용하여 나노섬유 웹을 제조한다.
Specifically, an aqueous solution of silver nitrate is placed in an aqueous solution of apatite and subjected to ultrasonic treatment for 20 to 40 minutes using a probe type ultrasonic disperser. After the sonication is complete, the solution is filtered and freeze-dried to prepare silver-apatite hydroxide particles. The prepared silver hydroxide apatite particles are dispersed at 1 to 5% by weight in the spinning solution in which the polymer is dissolved, and a nanofiber web is prepared using a known electrospinning method.
본 발명에서 제조된 나노섬유 웹의 항균성 시험은 아래의 방법으로 실시하였다.The antimicrobial test of the nanofiber web prepared in the present invention was carried out by the following method.
항균성 시험은 KS J 4206:2008 항균기능 제품의 항균력 시험 방법에 의하여 진탕플라스크법으로 시험하였다. 시료와 균 배양액을 접촉시켜 배양하고 CFU (Colony forming unit)을 측정하여 항균성을 평가하였다. 공시균으로는 Escherichia coli (ATCC 25922), Staphylococcus aureus (ATCC 6538) 및 Klebsiella pneumoniae (ATCC 4352)를 각각 사용하였다. 뉴트리언트 배지로는 Bacto-peptone 5g, Beef extract 3g, 증류수 1,000 ml, pH 6.8±0.2 (25℃)의 조건을 사용하였다. 항균성은 항균가공시료와 대조시료에 공시균을 접종하고 배양 후, 생균수를 측정하여 항균가공시료와 대조시료의 균수를 비교하는 정균감소율을 다음 식을 이용하여 구하여 평가하였다.The antimicrobial test was conducted by shaking flask method according to the antimicrobial activity test method of KS J 4206: 2008 antimicrobial function product. The culture was contacted with the sample and the culture medium and the CFU (Colony forming unit) was measured to evaluate the antimicrobial activity. Escherichia coli (ATCC 25922), Staphylococcus aureus (ATCC 6538) and Klebsiella pneumoniae (ATCC 4352) were used as test bacteria. As a nutrient medium, Bacto-peptone 5g, Beef extract 3g, 1,000 ml of distilled water, pH 6.8 ± 0.2 (25 ℃) was used. Antimicrobial activity was evaluated by inoculating the microorganisms in the antimicrobial and control samples, and incubating the cells.
Ma : 대조 시료의 접종 직후(초기) 균수 (평균값)M a : Number of bacteria immediately after inoculation of the control sample (initial value) (average value)
Mb : 24시간 배양 후 대조 시료의 균수 (평균값)M b : Number of bacteria in control sample after incubation for 24 hours (average value)
Mc : 24시간 배양 후 시험 시료의 균수 (평균값)
M c : Number of bacteria in the test sample after 24 hours incubation (average value)
이하에서는 실시예를 들어서 본 발명을 상세하게 설명하지만, 아래의 실시예에 의하여 본 발명의 권리범위가 제한되는 것은 아니다.
Hereinafter, the present invention will be described in detail with reference to Examples, but the scope of the present invention is not limited by the following Examples.
실시예Example 1 One
디메틸포름아미드(DMF) 85g에 수산화아파타이트(HAp) 0.15g을 넣고 프로브타입의 초음파 분산기(sonicator)로 30분간 분산시켰다. 상기 분산용액에 폴리아크릴로니트릴(PAN)을 14.85g을 용해시켜서 균일한 복합용액을 제조하고, 전기방사법을 이용하여 섬유직경이 0.5 내지 1㎛인 나노섬유 웹을 제조하였다. 제조된 나노섬유웹을 100ppm의 질산은(AgNO3) 수용액에 10분간 침지하여 음이온을 흡착 및 담지시켜서 은-나노섬유 웹을 제조하였다. 제조된 은-나노섬유 웹의 항균성을 측정하여 표 1에 나타내었다. 또한 제조된 나노섬유웹의 EDS 스펙트럼을 도 2에 나타내었다. 도 2를 보면, 나노섬유 웹에 은이온이 존재하는 것을 알 수 있다.
0.15 g of apatite hydroxide (HAp) was added to 85 g of dimethylformamide (DMF), followed by dispersion for 30 minutes with a probe-type ultrasonic sonicator. 14.85 g of polyacrylonitrile (PAN) was dissolved in the dispersion solution to prepare a uniform composite solution, and a nanofiber web having a fiber diameter of 0.5 to 1 μm was prepared by electrospinning. The prepared nanofiber web was immersed in 100 ppm of silver nitrate (AgNO 3 ) solution for 10 minutes to adsorb and support anions to prepare a silver-nanofiber web. Table 1 shows the antimicrobial activity of the prepared silver-nanofiber webs. In addition, the EDS spectrum of the prepared nanofiber web is shown in FIG. 2, it can be seen that silver ions are present in the nanofiber web.
실시예Example 2 2
수산화아파타이트(HAp)를 0.75g, 폴리아크릴로니트릴을 14.25g을 사용한 것 이외에는 실시예 1과 동일한 방법으로 은-나노섬유 웹을 제조하였다. 제조된 은-나노섬유 웹의 항균성을 측정하여 표 1에 나타내었다.
A silver-nanofiber web was prepared in the same manner as in Example 1 except that 0.75 g of apatite hydroxide (HAp) and 14.25 g of polyacrylonitrile were used. Table 1 shows the antimicrobial activity of the prepared silver-nanofiber webs.
실시예Example 3 3
수산화아파타이트(HAp)를 1.5g, 폴리아크릴로니트릴을 13.5g을 사용한 것 이외에는 실시예 1과 동일한 방법으로 은-나노섬유 웹을 제조하였다. 제조된 은-나노섬유 웹의 항균성을 측정하여 표 1에 나타내었다.
A silver-nanofiber web was prepared in the same manner as in Example 1 except that 1.5 g of apatite hydroxide (HAp) and 13.5 g of polyacrylonitrile were used. Table 1 shows the antimicrobial activity of the prepared silver-nanofiber webs.
실시예Example 4 4
수산화아파타이트(HAp)를 3g, 폴리아크릴로니트릴을 12g을 사용한 것 이외에는 실시예 1과 동일한 방법으로 은-나노섬유 웹을 제조하였다. 제조된 은-나노섬유 웹의 항균성을 측정하여 표 1에 나타내었다. 또한 제조된 나노섬유웹의 SEM 사진을 도 1에 나타내었다.
A silver-nanofiber web was prepared in the same manner as in Example 1 except that 3 g of apatite hydroxide (HAp) and 12 g of polyacrylonitrile were used. Table 1 shows the antimicrobial activity of the prepared silver-nanofiber webs. In addition, the SEM image of the prepared nanofiber web is shown in FIG.
함량HAp
content
Claims (6)
상기 수산화아파타이트를 분산시킨 분산용액에 고분자를 용해시켜서 방사용액을 제조하는 단계;
상기 방사용액을 전기방사하여 나노섬유 웹을 제조하는 단계; 및
상기 나노섬유 웹을 질산은 수용액에 침지하여 은이온을 흡착 및 담지시키는 단계를 포함하는 것을 특징으로 하는 항균성이 우수한 나노섬유 웹의 제조방법.In the manufacturing method of the nanofiber web excellent in antimicrobial containing apatite hydroxide and silver,
Preparing a spinning solution by dissolving a polymer in a dispersion solution in which the apatite hydroxide is dispersed;
Preparing a nanofiber web by electrospinning the spinning solution; And
And immersing the nanofiber web in an aqueous solution of silver nitrate to adsorb and support silver ions.
상기 수산화아파타이트는 방사용액 중량 대비 0.1 내지 5중량% 포함되어 있는 것을 특징으로 하는 항균성이 우수한 나노섬유 웹의 제조방법.The method according to claim 2,
The method of producing a nanofiber web excellent antimicrobial, characterized in that the apatite hydroxide is contained 0.1 to 5% by weight relative to the weight of the spinning solution.
질산은 수용액에 수산화아파타이트를 넣고 분산시켜 분산액을 제조하는 단계;
상기 분산액을 동결 및 건조하여 은-수산화아파타이트 복합체를 제조하는 단계;
상기 복합체를 고분자 용액에 방사용액 총 중량대비 1 내지 5중량% 첨가하여 방사용액을 제조하는 단계; 및
상기 방사용액을 전기방사하여 나노섬유 웹을 제조하는 단계를 포함하는 것을 특징으로 하는 항균성이 우수한 나노섬유 웹의 제조방법.In the manufacturing method of the nanofiber web excellent in antimicrobial containing apatite hydroxide and silver,
Preparing a dispersion by adding and dispersing apatite in an aqueous silver nitrate solution;
Freezing and drying the dispersion to prepare a silver hydroxide apatite complex;
Preparing a spinning solution by adding 1 to 5 wt% of the complex to the polymer solution based on the total weight of the spinning solution; And
Electrospinning the spinning solution to produce a nanofiber web, characterized in that it comprises a step of producing a nanofiber web.
상기 수산화아파타이트는 프로브형 초음파 분산기를 사용하여 20~40분간 분산시킨 것을 특징으로 하는 항균성이 우수한 나노섬유 웹의 제조방법.The method according to claim 2 or 4,
The method of producing a nanofiber web excellent antibacterial, characterized in that the apatite hydroxide is dispersed for 20 to 40 minutes using a probe-type ultrasonic disperser.
상기 고분자는 폴리아크릴로니트릴, 폴리비닐알코올 및 폴리우레탄으로 이루어진 군에서 선택된 1종인 것을 특징으로 하는 항균성이 우수한 나노섬유 웹의 제조방법.The method according to claim 2 or 4,
The polymer is a method of producing a nanofiber web with excellent antimicrobial properties, characterized in that one selected from the group consisting of polyacrylonitrile, polyvinyl alcohol and polyurethane.
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| CN111235875B (en) * | 2019-10-14 | 2021-12-28 | 四川大学 | Silver-plated special-shaped polyvinyl alcohol fiber, and preparation method and application thereof |
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