KR102053668B1 - Anti-microbial and Ultraviolet Protective fibers and method of manufacturing the same - Google Patents
Anti-microbial and Ultraviolet Protective fibers and method of manufacturing the same Download PDFInfo
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- KR102053668B1 KR102053668B1 KR1020130121513A KR20130121513A KR102053668B1 KR 102053668 B1 KR102053668 B1 KR 102053668B1 KR 1020130121513 A KR1020130121513 A KR 1020130121513A KR 20130121513 A KR20130121513 A KR 20130121513A KR 102053668 B1 KR102053668 B1 KR 102053668B1
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- fiber
- zinc oxide
- silver
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- 239000000835 fiber Substances 0.000 title claims abstract description 93
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 18
- 230000000845 anti-microbial effect Effects 0.000 title abstract description 10
- 239000004599 antimicrobial Substances 0.000 title abstract description 4
- 230000001681 protective effect Effects 0.000 title 1
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims abstract description 72
- 239000002245 particle Substances 0.000 claims abstract description 44
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims abstract description 34
- 229910052709 silver Inorganic materials 0.000 claims abstract description 32
- 239000004332 silver Substances 0.000 claims abstract description 32
- 239000002131 composite material Substances 0.000 claims abstract description 31
- 239000011342 resin composition Substances 0.000 claims abstract description 28
- 239000000243 solution Substances 0.000 claims abstract description 21
- 238000002256 photodeposition Methods 0.000 claims abstract description 14
- 239000007864 aqueous solution Substances 0.000 claims abstract description 13
- 239000002105 nanoparticle Substances 0.000 claims abstract description 12
- 239000011858 nanopowder Substances 0.000 claims abstract description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229910021645 metal ion Inorganic materials 0.000 claims abstract description 8
- 239000011787 zinc oxide Substances 0.000 claims description 17
- 238000000034 method Methods 0.000 claims description 15
- 239000004677 Nylon Substances 0.000 claims description 14
- 229920001778 nylon Polymers 0.000 claims description 14
- 229920005989 resin Polymers 0.000 claims description 14
- 239000011347 resin Substances 0.000 claims description 14
- 239000000203 mixture Substances 0.000 claims description 7
- 229910052751 metal Inorganic materials 0.000 claims description 5
- 239000002184 metal Substances 0.000 claims description 5
- 150000001875 compounds Chemical class 0.000 claims description 3
- 238000007654 immersion Methods 0.000 claims description 3
- 238000009281 ultraviolet germicidal irradiation Methods 0.000 claims description 3
- 238000002074 melt spinning Methods 0.000 claims description 2
- 239000002243 precursor Substances 0.000 claims 2
- 238000001523 electrospinning Methods 0.000 claims 1
- 230000001678 irradiating effect Effects 0.000 claims 1
- 230000003287 optical effect Effects 0.000 claims 1
- 239000012266 salt solution Substances 0.000 claims 1
- 150000003839 salts Chemical group 0.000 claims 1
- 238000009987 spinning Methods 0.000 abstract description 33
- 239000010931 gold Substances 0.000 abstract description 29
- 239000010949 copper Substances 0.000 abstract description 20
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 abstract description 19
- 229910052737 gold Inorganic materials 0.000 abstract description 19
- 229920005992 thermoplastic resin Polymers 0.000 abstract description 19
- 230000000903 blocking effect Effects 0.000 abstract description 15
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 abstract description 10
- 229910052802 copper Inorganic materials 0.000 abstract description 10
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 abstract description 9
- 230000000844 anti-bacterial effect Effects 0.000 abstract description 5
- 239000004408 titanium dioxide Substances 0.000 abstract description 4
- 239000002114 nanocomposite Substances 0.000 abstract 2
- 230000001877 deodorizing effect Effects 0.000 abstract 1
- 239000000463 material Substances 0.000 abstract 1
- 229910044991 metal oxide Inorganic materials 0.000 abstract 1
- 150000004706 metal oxides Chemical class 0.000 abstract 1
- 239000004065 semiconductor Substances 0.000 abstract 1
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 18
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 description 16
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Substances [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 9
- 238000002156 mixing Methods 0.000 description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 8
- 239000012153 distilled water Substances 0.000 description 6
- 238000002149 energy-dispersive X-ray emission spectroscopy Methods 0.000 description 6
- 239000002952 polymeric resin Substances 0.000 description 6
- 239000000843 powder Substances 0.000 description 6
- 229910001961 silver nitrate Inorganic materials 0.000 description 6
- 229920003002 synthetic resin Polymers 0.000 description 6
- 239000004594 Masterbatch (MB) Substances 0.000 description 5
- 229920000728 polyester Polymers 0.000 description 5
- 101710134784 Agnoprotein Proteins 0.000 description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- 210000002268 wool Anatomy 0.000 description 4
- WFDIJRYMOXRFFG-UHFFFAOYSA-N Acetic anhydride Chemical compound CC(=O)OC(C)=O WFDIJRYMOXRFFG-UHFFFAOYSA-N 0.000 description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
- 238000001125 extrusion Methods 0.000 description 3
- -1 polypropylene Polymers 0.000 description 3
- BJEPYKJPYRNKOW-REOHCLBHSA-N (S)-malic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O BJEPYKJPYRNKOW-REOHCLBHSA-N 0.000 description 2
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 2
- BJEPYKJPYRNKOW-UHFFFAOYSA-N alpha-hydroxysuccinic acid Natural products OC(=O)C(O)CC(O)=O BJEPYKJPYRNKOW-UHFFFAOYSA-N 0.000 description 2
- 230000003373 anti-fouling effect Effects 0.000 description 2
- 238000000635 electron micrograph Methods 0.000 description 2
- 235000011090 malic acid Nutrition 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- 210000004243 sweat Anatomy 0.000 description 2
- 239000011032 tourmaline Substances 0.000 description 2
- 229940070527 tourmaline Drugs 0.000 description 2
- 229910052613 tourmaline Inorganic materials 0.000 description 2
- 229910052726 zirconium Inorganic materials 0.000 description 2
- BJEPYKJPYRNKOW-UWTATZPHSA-N (R)-malic acid Chemical compound OC(=O)[C@H](O)CC(O)=O BJEPYKJPYRNKOW-UWTATZPHSA-N 0.000 description 1
- 241000588747 Klebsiella pneumoniae Species 0.000 description 1
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 1
- 239000004952 Polyamide Substances 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
- 239000004743 Polypropylene Substances 0.000 description 1
- 239000004372 Polyvinyl alcohol Substances 0.000 description 1
- FOIXSVOLVBLSDH-UHFFFAOYSA-N Silver ion Chemical compound [Ag+] FOIXSVOLVBLSDH-UHFFFAOYSA-N 0.000 description 1
- 241000191967 Staphylococcus aureus Species 0.000 description 1
- 230000006750 UV protection Effects 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 1
- 239000004327 boric acid Substances 0.000 description 1
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 description 1
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 1
- 239000000292 calcium oxide Substances 0.000 description 1
- 229920002301 cellulose acetate Polymers 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 230000009477 glass transition Effects 0.000 description 1
- 238000007733 ion plating Methods 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 229940116298 l- malic acid Drugs 0.000 description 1
- 239000012803 melt mixture Substances 0.000 description 1
- 239000011812 mixed powder Substances 0.000 description 1
- 238000005240 physical vapour deposition Methods 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 229920000747 poly(lactic acid) Polymers 0.000 description 1
- 229920002239 polyacrylonitrile Polymers 0.000 description 1
- 229920002647 polyamide Polymers 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 239000004626 polylactic acid Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 229920000193 polymethacrylate Polymers 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 229920002689 polyvinyl acetate Polymers 0.000 description 1
- 239000011118 polyvinyl acetate Substances 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 230000004224 protection Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 229920002994 synthetic fiber Polymers 0.000 description 1
- 239000012209 synthetic fiber Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 150000003609 titanium compounds Chemical class 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- XROWMBWRMNHXMF-UHFFFAOYSA-J titanium tetrafluoride Chemical compound [F-].[F-].[F-].[F-].[Ti+4] XROWMBWRMNHXMF-UHFFFAOYSA-J 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
- 239000002759 woven fabric Substances 0.000 description 1
Images
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- 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
-
- 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
- D01D1/00—Treatment of filament-forming or like material
- D01D1/06—Feeding liquid to the spinning head
- D01D1/065—Addition and mixing of substances to the spinning solution or to the melt; Homogenising
-
- 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
- D01D5/28—Formation of filaments, threads, or the like while mixing different spinning solutions or melts during the spinning operation; Spinnerette packs therefor
- D01D5/30—Conjugate filaments; Spinnerette packs therefor
- D01D5/34—Core-skin structure; Spinnerette packs therefor
-
- 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
-
- 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
- D01F1/106—Radiation shielding agents, e.g. absorbing, reflecting agents
-
- D—TEXTILES; PAPER
- D02—YARNS; MECHANICAL FINISHING OF YARNS OR ROPES; WARPING OR BEAMING
- D02G—CRIMPING OR CURLING FIBRES, FILAMENTS, THREADS, OR YARNS; YARNS OR THREADS
- D02G3/00—Yarns or threads, e.g. fancy yarns; Processes or apparatus for the production thereof, not otherwise provided for
- D02G3/44—Yarns or threads characterised by the purpose for which they are designed
- D02G3/441—Yarns or threads with antistatic, conductive or radiation-shielding properties
-
- D—TEXTILES; PAPER
- D02—YARNS; MECHANICAL FINISHING OF YARNS OR ROPES; WARPING OR BEAMING
- D02G—CRIMPING OR CURLING FIBRES, FILAMENTS, THREADS, OR YARNS; YARNS OR THREADS
- D02G3/00—Yarns or threads, e.g. fancy yarns; Processes or apparatus for the production thereof, not otherwise provided for
- D02G3/44—Yarns or threads characterised by the purpose for which they are designed
- D02G3/449—Yarns or threads with antibacterial properties
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M10/00—Physical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. ultrasonic, corona discharge, irradiation, electric currents, or magnetic fields; Physical treatment combined with treatment with chemical compounds or elements
- D06M10/001—Treatment with visible light, infrared or ultraviolet, X-rays
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/10—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing oxygen
- D06M13/144—Alcohols; Metal alcoholates
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
- D06M2200/25—Resistance to light or sun, i.e. protection of the textile itself as well as UV shielding materials or treatment compositions therefor; Anti-yellowing treatments
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- D—TEXTILES; PAPER
- D10—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
- D10B—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
- D10B2401/00—Physical properties
- D10B2401/13—Physical properties anti-allergenic or anti-bacterial
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- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Mechanical Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Artificial Filaments (AREA)
Abstract
본 발명은 항균 기능과 자외선 차단 기능을 가지는 섬유 및 이의 제조방법에 관한 것이다. 본 발명에 따른 항균 및 자외선 차단 기능을 가지는 섬유 및 이의 제조방법은 구체적으로 5 마이크로 이하의 산화아연(ZnO) 나노분말을 0.5~20중량%와 열가소성 수지 80~99.5중량%를 함유하는 수지 조성물을 방사하여 섬유를 제조하는 방법 또는 5 마이크로 이하의 산화아연(ZnO) 나노분말을 0.5~20중량%와 열가소성 수지 80~99.5중량%를 함유하는 수지 조성물을 복합방사 섬유의 초부(sheath)를 형성하고 열가소성 수지가 심부(core)를 형성하는 복합섬유를 제조한 후 상기 섬유를 은(Ag), 금(Pt), 금(Au), 구리(Cu) 등의 금속이온 수용액과 알콜로 이루어진 용액에 침지후 광증착(photodeposition)시켜 이산화티탄 입자 함유 복합 방사한 섬유의 이산화티탄 입자 위에 은(Ag), 금(Pt), 금(Au), 구리(Cu) 등 나노입자가 담지된 기능성 나노 복합섬유를 제조한다. 본 발명의 기능성 나노복합 섬유는 은(Ag), 금(Pt), 금(Au), 구리(Cu) 등 나노입자가 담지된 반도체 금속산화물 입자를 함유한 기능성 복합 섬유로 자외선 차단, 전자파차폐, 방취 및 항균성 소재 등으로 활용 가능하다.The present invention relates to a fiber having an antibacterial function and an ultraviolet ray blocking function and a method of manufacturing the same. Fiber having an antimicrobial and ultraviolet ray blocking function and a method for producing the same according to the present invention specifically comprises a resin composition containing 0.5 to 20% by weight of zinc oxide (ZnO) nanopowder of 5 microns or less and 80 to 99.5% by weight of a thermoplastic resin. Spinning to form a fiber or a resin composition containing 0.5 to 20% by weight of zinc oxide (ZnO) nanopowder of 5 microns or less and 80 to 99.5% by weight of a thermoplastic resin to form the sheath of the composite spun fiber After preparing a composite fiber in which a thermoplastic resin forms a core, the fiber is immersed in a solution consisting of an aqueous solution of a metal ion such as silver (Ag), gold (Pt), gold (Au), copper (Cu) and an alcohol. The functional nano-composite fiber in which nanoparticles such as silver (Ag), gold (Pt), gold (Au) and copper (Cu) are supported on the titanium dioxide particles of the composite spun fiber containing titanium dioxide particles by photodeposition Manufacture. The functional nanocomposite fiber of the present invention is a functional composite fiber containing semiconductor metal oxide particles on which nanoparticles such as silver (Ag), gold (Pt), gold (Au), copper (Cu), etc. are supported. It can be used as deodorizing and antimicrobial materials.
Description
본 발명은 항균 기능과 자외선 차단 기능을 가지는 섬유 및 이의 제조방법에 관한 것이다. The present invention relates to a fiber having an antibacterial function and an ultraviolet ray blocking function and a method of manufacturing the same.
본 발명은 항균 기능과 자외선 차단 기능을 가지는 섬유 및 이의 제조방법에 관한 것이다. 본 발명에 따른 항균 및 자외선 차단 기능을 가지는 섬유 및 이의 제조방법은 구체적으로 5 마이크로 이하의 산화아연(ZnO) 나노분말을 0.5~20중량%와 열가소성 수지 80~99.5중량%를 함유하는 수지 조성물을 방사하여 섬유를 제조하는 방법 또는 5 마이크로 이하의 산화아연(ZnO) 나노분말을 0.5~20중량%와 열가소성 수지 80~99.5중량%를 함유하는 수지 조성물을 복합방사 섬유의 초부(sheath)를 형성하고 열가소성 수지가 심부(core)를 형성하는 복합섬유를 제조한 후 상기 섬유를 은(Ag), 금(Pt), 금(Au), 구리(Cu) 등의 금속이온 수용액과 알콜로 이루어진 용액에 침지후 광증착(photodeposition)시켜 산화아연 입자 함유 복합 방사한 섬유의 산화아연 입자 위에 은(Ag), 금(Pt), 금(Au), 구리(Cu) 등 나노 입자가 담지된 기능성 복합섬유를 제조한다.The present invention relates to a fiber having an antibacterial function and an ultraviolet ray blocking function and a method of manufacturing the same. Fiber having an antimicrobial and ultraviolet ray blocking function and a method for producing the same according to the present invention specifically comprises a resin composition containing 0.5 to 20% by weight of zinc oxide (ZnO) nanopowder of 5 microns or less and 80 to 99.5% by weight of a thermoplastic resin. Spinning to form a fiber or a resin composition containing 0.5 to 20% by weight of zinc oxide (ZnO) nanopowder of 5 microns or less and 80 to 99.5% by weight of a thermoplastic resin to form the sheath of the composite spun fiber After preparing a composite fiber in which a thermoplastic resin forms a core, the fiber is immersed in a solution consisting of an aqueous solution of a metal ion such as silver (Ag), gold (Pt), gold (Au), copper (Cu) and an alcohol. After the photodeposition to produce functional composite fibers in which nanoparticles such as silver (Ag), gold (Pt), gold (Au) and copper (Cu) are supported on the zinc oxide particles of the composite spun fiber containing zinc oxide particles. do.
대한민국 특허 10-1157513호에서는 표면에 10 내지 100nm 두께로 은(Ag) 나노 입자가 불규칙하게 증착된 폴리에스테르 마스터배치 칩을 이용하여 제조된다. 또한, 본 발명에 따른 다기능사는 은 나노 입자를 원료인 폴리에스테르 마스터배치 표면에 불규칙하고 불연속적으로 증착하여 원사 제조과정에서 은 나노 입자가 쉽게 탈락되지 않기 때문에 상기 항균성이 반영구적으로 지속되며, 모노필라멘트의 단면이 삼엽상인 이형단면사로 제조되므로 땀이나 수분 등의 흡수와 배출이 용이하게 이루어져서 흡한 속건성을 부여하는 다기능 섬유의 제조방법이 있으며 대한민국 공개특허 10-2004-0098808호에서는 폴리프로필렌 수지에 평균입경 0.3 아이크로 메타정도의 이산화티탄 분말, 토루말린 분말, 세리사이트 분말, 은분말, 실리카, 산화칼슘, 산화아연, 지루코늄 등의 혼합문말을 일정비율로 첨가한 조성물을 만들어 폴리프로필렌 수지와 3: 2의 중량비로 혼합하여 마스터배치를 만들고 이를 다시 폴리프로필렌 수지와 5:5의 중량비로 혼합하여 120~140℃에서 1시간정도 열처리하여 수분과 습기를 제거한 후 220~240℃에서 용융방사하는 것을 특징으로 하는 항균, 정화, 방오, 자외선 차단, 원적외선, 전자파차단 기능을 가지는 폴리프로필렌 멀티 필라멘트사 및 그의 제조하는 기술이 있으며 또한 대한민국 공개특허 10-2001-0012855호에서는 DMF(90중량%)에 무수초산(10중량%)을 용해한 용액에 전정련한 양모를 침지하고, 50℃까지 승온시켜 이 온도를 30분간 유지하여 음이온화 처리를 행하고, 그 후, 양모를 물에 씻는다. 한편, 티탄알콕시드 및 플루오르화티탄중 적어도 하나의 티탄 화합물을 2.0% owf의 비율로 용해한다. 이 수용액에 음이온화 처리한 양모를 침지시키고, 상온에서 30분간 처리한다. 이어서, 붕산 : 시트르산 : D, L-말산 = 0.5 : 1 : 1의 중량비율로 혼합한 것을 상기 수용액에 0.5%owf의 비율로 첨가하여, 50℃에서 30분간 처리하고, 그 후, 물에 씻음으로써, 섬유표면이 산화티탄으로 도금된 천연섬유를 제조함으로서 기능성을 부여하고자 하는 시도들이 존재하고 있다.상기의 방법 중 대한민국 특허 10-1157513호에서는 폴리에스테르 마스터배치 칩을 화학기상증착법, 또는 직류/교류 스퍼터링 및 이온 플레이팅과 같은 물리 기상증착법을 사용하기 때문에 고가의 진공장비를 사용하여서 제조하여야 하는 단점이 있으며 10-2004-0098808호의 경우는 항균, 정화, 방오, 자외선차단, 전자파차단 기능을 가지는 섬유를 제조하기 위해서는 이산화티타늄분말, 토르말린 분말,은분말, 실리카, 지르코늄 등의 복잡한 혼합 분말을 고분자 수지에 혼련해야하는 제약이 있으며 대한민국 공개특허 10-2001-0012855호의 경우는 양모 등 천연섬유에 기술이 적용이 가능하며 합성섬유의 경우에는 적용에 제약이 따른다. 이러한 방법들과는 달리 본 발명에서는 5 마이크로 이하의 산화아연(ZnO) 나노분말을 0.5~20중량%와 열가소성 수지 80~99.5중량%를 함유하는 수지 조성물을 방사하여 섬유를 제조하는 방법 또는 5 마이크로 이하의 산화아연(ZnO) 분말을 0.5~20중량%와 열가소성 수지 80~99.5중량%를 함유하는 수지 조성물을 복합방사 섬유의 초부(sheath)를 형성하고 열가소성 수지가 심부(core)를 형성하는 복합섬유를 제조한 후 상기 섬유들을 은(Ag), 금(Pt), 금(Au), 구리(Cu) 등의 금속이온 수용액과 알콜로 이루어진 용액에 침지후 광증착(photodeposition)시켜 산화아연 입자 함유 복합 방사한 섬유의 산화아연 입자 위에 은(Ag), 금(Pt), 금(Au), 구리(Cu) 등 나노입자가 담지된 기능성 복합섬유를 제조한다. 본 방법은 고분자의 종류에 상관없이 은(Ag), 백금(Pt), 금(Au), 구리(Cu) 등의 나노입자를 선택적으로 담지할 수 있는 장점이 있으며 항균, 자외선 차단, 소취 등의 다기능성을 가지는 기능성을 가지게 한다.Korean Patent 10-1157513 is prepared using a polyester masterbatch chip in which silver (Ag) nanoparticles are irregularly deposited to a thickness of 10 to 100nm on the surface. In addition, the multifunctional yarn according to the present invention is semi-permanently deposited on the surface of the polyester masterbatch of the raw material is irregular and discontinuous, so the silver nanoparticles are not easily dropped during the yarn manufacturing process, the antimicrobial persists semi-permanently, monofilament Since the cross-section of the three-sided shape is made of a cross-section yarn is easy to absorb and discharge sweat or moisture, there is a manufacturing method of a multi-functional fiber that gives a quick-drying sweat absorption in Korea Patent Publication No. 10-2004-0098808 A composition containing a mixture of titanium dioxide powder, tourmaline powder, sericite powder, silver powder, silica, calcium oxide, zinc oxide, zirconium, etc., having a particle size of 0.3 micrometer, in a proportion, was prepared. : Mix by weight ratio of 2 and make masterbatch Antibacterial, purifying, antifouling, UV blocking, far infrared rays, electromagnetic wave blocking, characterized in that the mixture is mixed at a weight ratio of 5: 5 and heat treated at 120 to 140 ° C. for 1 hour to remove moisture and moisture, followed by melt spinning at 220 to 240 ° C. There is a polypropylene multifilament yarn having a function and a technique for manufacturing the same, and in Korea Patent Publication No. 10-2001-0012855 also immersed pre-refined wool in a solution dissolved in acetic anhydride (10% by weight) in DMF (90% by weight). Then, the temperature is raised to 50 ° C, the temperature is maintained for 30 minutes, anionization treatment is performed, and the wool is then washed with water. On the other hand, at least one titanium compound of titanium alkoxide and titanium fluoride is dissolved at a rate of 2.0% owf. The anionized wool is immersed in this aqueous solution and treated at room temperature for 30 minutes. Subsequently, a mixture of boric acid: citric acid: D and L-malic acid = 0.5: 1: 1 was added to the aqueous solution at a rate of 0.5% owf, and treated at 50 ° C for 30 minutes, and then washed with water. Attempts have been made to impart functionality by producing natural fibers coated with titanium oxide on the surface of the fiber. Among the above methods, Korean Patent No. 10-1157513 discloses that a polyester masterbatch chip is used for chemical vapor deposition or direct current / Due to the use of physical vapor deposition methods such as AC sputtering and ion plating, it has to be manufactured using expensive vacuum equipment. In case of 10-2004-0098808, it has antibacterial, purifying, antifouling, UV blocking and electromagnetic blocking functions. In order to manufacture fibers, complex mixed powders such as titanium dioxide powder, tourmaline powder, silver powder, silica and zirconium must be kneaded into a polymer resin. There are about the arc when 10-2001-0012855 Republic of Korea Patent Publication is capable of this technique applied to natural fibers such as wool and it follows in the case of synthetic fiber, the constraints on the application. Unlike these methods, in the present invention, a method of preparing fibers by spinning a resin composition containing 0.5 to 20% by weight of zinc oxide (ZnO) nanopowder of 5 microns or less and 80 to 99.5% by weight of thermoplastic resin, or 5 microns or less A resin composition containing 0.5 to 20% by weight of zinc oxide (ZnO) powder and 80 to 99.5% by weight of thermoplastic resin is used to form a composite fiber in which a sheath of the composite spun fiber is formed and the thermoplastic resin forms a core. After fabrication, the fibers are immersed in a solution consisting of an aqueous solution of metal ions such as silver (Ag), gold (Pt), gold (Au), copper (Cu) and alcohol, followed by photodeposition of zinc oxide particles containing composite spinning Functional composite fibers in which nanoparticles such as silver (Ag), gold (Pt), gold (Au), copper (Cu) and the like are supported on zinc oxide particles of one fiber are prepared. This method has the advantage of selectively supporting nanoparticles such as silver (Ag), platinum (Pt), gold (Au) and copper (Cu) regardless of the type of polymer. Let's have functionality with multifunctionality.
본 발명의 일 구현예는, 5㎛ 이하의 산화아연(ZnO) 나노분말을 0.5~20중량%와 열가소성 수지 80~99.5중량%를 함유하는 수지 조성물을 함유하는 섬유를 제조한 후 상기 섬유를 은(Ag)을 함유하는 금속이온 수용액과 알콜로 이루어진 용액에 침지후 UV 조사로 광증착(photodeposition)시켜 산화아연 입자 함유 섬유의 산화아연 입자 위에 은(Ag) 나노 입자가 담지된 기능성 섬유 및 제조할 수 있는 방법을 제공한다. One embodiment of the present invention, after preparing a fiber containing a resin composition containing 0.5 to 20% by weight of zinc oxide (ZnO) nanopowder of 5㎛ or less and 80 to 99.5% by weight of the thermoplastic resin is silver Functional fibers in which silver (Ag) nanoparticles are supported on zinc oxide particles of the zinc oxide particle-containing fiber by photodeposition by UV irradiation after immersion in a solution consisting of an aqueous metal ion solution containing (Ag) and an alcohol. It provides a way to do it.
이상에서 살펴본 바와 같이. 본 발명은 5㎛ 이하의 산화아연(ZnO) 나노분말을 0.5~20중량%와 열가소성 수지 80~99.5중량%를 함유하는 수지 조성물을 단독 방사하여 섬유를 제조하거나 복합방사 섬유의 초부(sheath)를 형성하고 열가소성 수지 조성물이 심부(core)를 형성하는 복합섬유를 제조한 후 상기 섬유를 은(Ag)을 함유하는 금속이온 수용액과 알콜로 이루어진 용액에 침지후 광증착(photodeposition)시켜 산화아연(ZnO) 입자를 함유하는 섬유의 산화아연(ZnO) 입자 위에 은(Ag) 나노 입자가 담지된 기능성 섬유를 제조할 수 있는 방법을 발명의 효과로 제공한다.As we have seen above. According to the present invention, a fiber composition is prepared by spinning a resin composition containing 0.5 to 20 wt% of zinc oxide (ZnO) nanopowder of 5 µm or less and 80 to 99.5 wt% of thermoplastic resin, or the sheath of the composite spun fiber After forming a composite fiber in which the thermoplastic resin composition forms a core, the fiber is immersed in a solution consisting of an aqueous metal ion solution containing alcohol (Ag) and alcohol and then photodepositioned to form zinc oxide (ZnO). The effect of the invention is to provide a method for producing functional fibers on which silver (Ag) nanoparticles are supported on zinc oxide (ZnO) particles of fibers containing particles).
도 1은 본 발명의 실시예 1, 2, 3에 사용된 산화아연 입자를 함유하는 섬유의 투사전자현미경(TEM) 사진이다.
도 2는 본 발명의 실시예 4, 5, 6에 사용된 산화아연 입자를 함유하는 초부와 심부로 이루어진 복합섬유의 투사전자현미경(TEM) 사진이다.
도 3은 본 발명의 실시예 1, 2, 3, 4, 5, 6의 복합섬유의 사진이다.
도 4는 본 발명의 실시예 1, 2, 3, 4, 5, 6의 복합섬유 표면의 전자현미경(SEM) 및 EDS 사진이다.
도 5는 본 발명의 실시예 1, 2, 3, 4, 5, 6의 복합섬유 직물의 XPS 분석 그림이다.1 is a projection electron microscope (TEM) photograph of a fiber containing zinc oxide particles used in Examples 1, 2, and 3 of the present invention.
FIG. 2 is a projection electron microscope (TEM) image of a composite fiber composed of a core part and a core part containing zinc oxide particles used in Examples 4, 5, and 6 of the present invention.
Figure 3 is a photograph of the composite fiber of Examples 1, 2, 3, 4, 5, 6 of the present invention.
Figure 4 is an electron microscope (SEM) and EDS photograph of the surface of the composite fiber of Examples 1, 2, 3, 4, 5, 6 of the present invention.
5 is an XPS analysis picture of the composite fiber fabrics of Examples 1, 2, 3, 4, 5, and 6 of the present invention.
상술하는 목적을 달성하기 위한 본 발명의 항균 및 자외선 차단 기능을 가지는 복합 섬유 및 이의 제조방법은 구체적으로 5 마이크로 이하의 산화아연(ZnO) 나노분말을 0.5~20중량%와 열가소성 수지 80~99.5중량%를 함유하는 수지 조성물을 방사하여 섬유를 제조하는 방법 또는 5 마이크로 이하의 산화아연(ZnO) 나노분말을 0.5~20중량%와 열가소성 수지 80~99.5중량%를 함유하는 수지 조성물을 복합방사 섬유의 초부(sheath)를 형성하고 열가소성 수지가 심부(core)를 형성하는 복합섬유 및 이의 제조방법이다. 이하 본 발명을 더욱 더 상세하게 설명한다. 먼저, 산화아연 입자를 열가소성 수지에 용융, 혼련하여 분산시켜 이들의 마스터 배치를 제조한다. 상기 제조된 마스터 배치는 방사하여 적용하거나 복합방사시 초부(sheath)에 적용된다. 심부를 형성하는 수지는 시판하는 일반 열가소성 수지로 적용가능하다. 상기 산화아연(ZnO) 입자는 2nm~5㎛ 이하의 시판하거나 합성하여 사용할 수 있다. 열가소성 수지로는 폴리아크릴로니트릴, 폴리비닐알콜, 폴리아미드, 폴리에스테르, 폴리젓산, 폴리에틸렌 옥사이드, 폴리에틸렌비닐알콜 공중합체, 셀룰로오스 아세테이트, 폴리메타크릴레이트, 폴리에스테르계 공중합체, 폴리비닐 아세테이트 등을 사용할 수 있다.In order to achieve the above object, the composite fiber having an antimicrobial and ultraviolet ray blocking function of the present invention and a method of manufacturing the same are specifically 0.5 to 20 wt% of zinc oxide (ZnO) nanopowder of 5 microns or less and 80 to 99.5 weight of a thermoplastic resin. A method of producing fibers by spinning a resin composition containing% or a resin composition containing 0.5 to 20% by weight of zinc oxide (ZnO) nanopowder of 5 microns or less and 80 to 99.5% by weight of thermoplastic resin. It is a composite fiber and a method of manufacturing the same that form the sheath (sheath) and the thermoplastic resin forms the core (core). Hereinafter, the present invention will be described in more detail. First, zinc oxide particles are melted, kneaded and dispersed in a thermoplastic resin to prepare their master batches. The prepared master batch is applied by spinning or sheath during compound spinning. The resin for forming the core portion is applicable to a commercially available general thermoplastic resin. The zinc oxide (ZnO) particles may be commercially available or synthesized with 2 nm to 5 μm or less. Examples of the thermoplastic resin include polyacrylonitrile, polyvinyl alcohol, polyamide, polyester, polylactic acid, polyethylene oxide, polyethylene vinyl alcohol copolymer, cellulose acetate, polymethacrylate, polyester copolymer, and polyvinyl acetate. Can be used.
상기 산화아연(ZnO) 입자를 고분자 수지에 용융 혼련하기 위하여 용융혼합기를 사용하여 100부의 고분자 수지에 중량비로 0.1부 내지 20부의 산화아연(ZnO) 입자를 첨가하여 고분자수지의 용융온도에서 완전한 혼합용융체가 될 때까지 혼합하여 각각 제조한다. 여기서 혼합기로서는 시그마믹서, 브라벤더, 싱글스크류 압출혼합기, 트윈스크류 압출혼합기, 컴파운더 등이 사용가능하며 기계적 혼합을 보다 효과적으로 수행하기 위해서는 컴파운더 및 트윈스크류 압출혼합기가 바람직하다.In order to melt-knead the zinc oxide (ZnO) particles into a polymer resin, a melt mixture is used to add 0.1 parts to 20 parts of zinc oxide (ZnO) particles in a weight ratio to 100 parts of the polymer resin, thereby completely mixing the molten metal at the melting temperature of the polymer resin. Each is mixed until it is prepared. Here, as a mixer, a sigma mixer, a brabender, a single screw extrusion mixer, a twin screw extrusion mixer, a compounder, etc. may be used, and in order to perform mechanical mixing more effectively, a compounder and a twin screw extrusion mixer are preferable.
상기 수지 조성물을 단독 방사 또는 복합 방사시에는 섬유의 초부(sheath)를형성하게 투입하고 열가소성 수지 조성물이 심부(core)를 형성하게 복합 방사장치에 투입하여 방사온도는 고분자 수지의 융점 근처에서 적정한 방사속도로 방사 또는 복합 방사하여 고분자수지의 유리전이 온도 근처의 적정한 온도에서 연신하여 제조 후 상기 섬유를 은(Ag), 금(Pt), 금(Au), 구리(Cu) 등의 금속이온 수용액과 알콜로 이루어진 용액에 침지 후 광증착(photodeposition)시켜 산화아연(ZnO) 입자 함유 섬유의 산화아연(ZnO) 입자 위에 은(Ag), 금(Pt), 금(Au), 구리(Cu) 등 나노 입자가 담지된 복합섬유를 제조한다.In the case of single spinning or composite spinning, the resin composition is added to form a sheath of fibers and the thermoplastic resin composition is introduced into a composite spinning device to form a core, and the spinning temperature is appropriately spun near the melting point of the polymer resin. After spinning or compound spinning at a suitable temperature near the glass transition temperature of the polymer resin, the fiber is prepared and the aqueous solution of metal ions such as silver (Ag), gold (Pt), gold (Au) and copper (Cu) After immersion in a solution made of alcohol, photodeposition is performed on the zinc oxide (ZnO) particles of the zinc oxide (ZnO) particles-containing fibers, such as silver (Ag), gold (Pt), gold (Au), and copper (Cu). The composite fiber bearing the particles is prepared.
이하, 실시예를 통하여 본 발명을 더욱 구체적으로 살펴본다. 그러나 본 발명은 하기 실시예에만 한정되는 것은 아니다.Hereinafter, the present invention will be described in more detail with reference to Examples. However, the present invention is not limited only to the following examples.
실시예에서 제조된 원사는 단독방사는 약 820d/10f 및 복합방사는 40d/24f로 제조하여 사용하였다.
The yarns produced in the examples were used to produce single yarns of about 820d / 10f and composite yarns of 40d / 24f.
[실시 예 1 ]Example 1
나일론 (Nylon) 수지에 대해 1중량부의 50nm 사이즈의 산화아연(ZnO)을 트윈스크류 컴파운더(Wrarner & Pfleiderer , Type ZSK 25)에 투입하고 온도 260℃ 내지 290℃에서 스크류속도 250 rpm, 토출량 l5kg/h로 혼합하여 수지조성물을 칩으로 만들었다. 산화아연(ZnO) 함유 수지조성물을 방사구멍 수가 10홀인 방사구금이 장착된 복합방사기에 투입한 다음 방사온도 280℃에서 권취속도 40m/분으로 방사한 후, 820데니어/10필라멘트의 섬유를 제조하였다. 상기 섬유의 단면은 도 1 투사전자현미경 사진에 산화아연 나노입자가 잘 분산된 상태를 보여진다. 상기 섬유를 1.5×10-3 mol 농도의 질산은(AgNO3) 수용액과 메탄올로 이루어진 용액에 침지한 상태에서 60초 동안 자외선 조사하여 광증착하였다. 광증착시 광원과의 거리를 5cm로 유지하고 상기 은(Ag)이 산화아연(ZnO) 입자상에 담지된 섬유를 증류수로 수세 후 상온 건조하였다. 도 3에서 은 입자가 광증착된 섬유의 사진을 보여주며, 도 4의 EDS 분석결과 및 도 5의 XPS 결과에서 알 수 있듯이 은 입자가 담지되어 있음을 알 수 있다.
1 part by weight of 50 nm zinc oxide (ZnO) is added to a twin screw compounder (Wrarner & Pfleiderer, Type ZSK 25) with respect to nylon resin. Mixing with h made the resin composition into chips. A zinc oxide (ZnO) -containing resin composition was introduced into a composite spinning machine equipped with spinnerets having 10 holes of spinning holes, and spun at a spinning speed of 40 m / min at a spinning temperature of 280 ° C., whereby 820 denier / 10 filament fibers were prepared. . The cross section of the fiber shows a state in which zinc oxide nanoparticles are well dispersed in a projection electron micrograph of FIG. 1. The fiber was photodeposited by ultraviolet irradiation for 60 seconds while immersing in a solution consisting of an aqueous solution of silver nitrate (AgNO 3) and methanol at a concentration of 1.5 × 10 −3 mol. At the time of photodeposition, the distance from the light source was maintained at 5 cm, and the fiber (Ag) supported on the zinc oxide (ZnO) particles was washed with distilled water and dried at room temperature. FIG. 3 shows a photograph of the fiber on which the silver particles are photo-deposited, and as can be seen from the EDS analysis result of FIG. 4 and the XPS result of FIG. 5, the silver particles are supported.
[실시 예 2 ]Example 2
나일론 (Nylon) 수지에 대해 1중량부의 50nm 사이즈의 산화아연(ZnO)을 트윈스크류 컴파운더(Wrarner & Pfleiderer , Type ZSK 25)에 투입하고 온도 260℃ 내지 290℃에서 스크류속도 250 rpm, 토출량 l5kg/h로 혼합하여 수지조성물을 칩으로 만들었다. 산화아연(ZnO) 함유 수지조성물을 방사구멍 수가 10홀인 방사구금이 장착된 복합방사기에 투입한 다음 방사온도 280℃에서 권취속도 40m/분으로 방사한 후, 820데니어/10필라멘트의 섬유를 제조하였다. 상기 섬유를 1.5×10-3 mol 농도의 질산은(AgNO3) 수용액과 메탄올로 이루어진 용액에 침지한 상태에서 120초 동안 자외선 조사하여 광증착하였다. 광증착시 광원과의 거리를 5cm로 유지하고 상기 은(Ag)이 산화아연(ZnO) 입자상에 담지된 섬유를 증류수로 수세 후 상온 건조하였다. 도 3에서 은 입자가 광증착된 섬유의 사진을 보여주며, 도 4의 EDS 분석결과 및 도 5의 XPS 결과에서 알 수 있듯이 은 입자가 담지되어 있음을 알 수 있다.
1 part by weight of 50 nm zinc oxide (ZnO) is added to a twin screw compounder (Wrarner & Pfleiderer, Type ZSK 25) with respect to nylon resin. Mixing with h made the resin composition into chips. A zinc oxide (ZnO) -containing resin composition was introduced into a composite spinning machine equipped with spinnerets having 10 holes of spinning holes, and spun at a spinning speed of 40 m / min at a spinning temperature of 280 ° C., whereby 820 denier / 10 filament fibers were prepared. . The fiber was photodeposited by ultraviolet irradiation for 120 seconds while immersing in a solution consisting of an aqueous solution of silver nitrate (AgNO3) and methanol at a concentration of 1.5 × 10 −3 mol. At the time of photodeposition, the distance from the light source was maintained at 5 cm, and the fiber (Ag) supported on the zinc oxide (ZnO) particles was washed with distilled water and dried at room temperature. FIG. 3 shows a photograph of the fiber on which the silver particles are photo-deposited, and as can be seen from the EDS analysis result of FIG. 4 and the XPS result of FIG. 5, the silver particles are supported.
[실시예 3 ]Example 3
나일론 (Nylon) 수지에 대해 1중량부의 50nm 사이즈의 산화아연(ZnO)을 트윈스크류 컴파운더(Wrarner & Pfleiderer , Type ZSK 25)에 투입하고 온도 260℃ 내지 290℃에서 스크류속도 250 rpm, 토출량 l5kg/h로 혼합하여 수지 조성물을 칩으로 만들었다. 산화아연(ZnO) 함유 수지 조성물을 방사구멍 수가 10홀인 방사구금이 장착된 복합방사기에 투입한 다음 방사온도 280℃에서 권취속도 40m/분으로 방사한 후, 820데니어/10필라멘트의 섬유를 제조하였다. 상기 섬유를 1.5×10-3 mol 농도의 질산은(AgNO3) 수용액과 메탄올로 이루어진 용액에 침지한 상태에서 180초 동안 자외선 조사하여 광증착하였다. 광증착시 광원과의 거리를 5cm로 유지하고 상기 은(Ag)이 산화아연(ZnO) 입자상에 담지된 섬유를 증류수로 수세 후 상온 건조하였다. 도 3에서 은 입자가 광증착된 섬유의 사진을 보여주며, 도 4의 EDS 분석결과 및 도 5의 XPS 결과에서 알 수 있듯이 은 입자가 담지되어 있음을 알 수 있다.
1 part by weight of 50 nm zinc oxide (ZnO) is added to a twin screw compounder (Wrarner & Pfleiderer, Type ZSK 25) with respect to nylon resin. Mixing with h made the resin composition into chips. A zinc oxide (ZnO) -containing resin composition was introduced into a multispinning spinner with a spinneret having 10 holes, and spun at a spinning speed of 40 m / min at a spinning temperature of 280 ° C., thereby producing 820 denier / 10 filament fibers. . The fiber was photodeposited by ultraviolet irradiation for 180 seconds while immersing in a solution consisting of an aqueous solution of silver nitrate (AgNO3) and methanol at a concentration of 1.5 × 10 −3 mol. At the time of photodeposition, the distance from the light source was maintained at 5 cm, and the fiber (Ag) supported on the zinc oxide (ZnO) particles was washed with distilled water and dried at room temperature. FIG. 3 shows a photograph of the fiber on which the silver particles are photo-deposited, and as can be seen from the EDS analysis result of FIG. 4 and the XPS result of FIG. 5, the silver particles are supported.
[실시예 4 ]Example 4
나일론 (Nylon) 수지에 대해 1중량부의 50nm 사이즈의 산화아연(ZnO)을 트윈스크류 컴파운더(Wrarner & Pfleiderer , Type ZSK 25)에 투입하고 온도 260℃ 내지 290℃에서 스크류속도 250 rpm, 토출량 l5kg/h로 혼합하여 수지 조성물을 칩으로 만들었다. 산화아연(ZnO) 함유 수지 조성물을 초부(sheath)에 투입하고 나일론(Nylon) 수지를 심부(core)에 투입하였다. 이때 S(초부)/C(심부)의 비는 5:5로 하였다. 방사구멍 수가 24홀인 방사구금이 장착된 복합방사기에 투입한 다음 방사온도 270℃에서 권취속도 4000m/분으로 방사한 후, 연신비 2로 연신하여 40데니어/24 필라멘트의 섬유를 제조하였다. 상기 섬유의 단면은 도 2의 투사전자현미경 사진에 산화아연 나노입자가 잘 분산된 상태를 보여주고 있으며 초부와 심부로 구성되어 있음을 알 수 있다. 상기 섬유를 1.5×10-4 mol 농도의 질산은(AgNO3) 수용액과 메탄올로 이루어진 용액에 침지한 상태에서 60초 동안 자외선 조사하여 광증착하였다. 광증착시 광원과의 거리를 5cm로 유지하고 상기 은(Ag)이 산화아연(ZnO) 입자상에 담지된 섬유를 증류수로 수세 후 상온 건조하였다. 도 3에서 은 입자가 광증착된 섬유의 사진을 보여주며, 도 4의 EDS 분석결과 및 도 5의 XPS 결과에서 알 수 있듯이 은 입자가 담지되어 있음을 알 수 있다.
1 part by weight of 50 nm zinc oxide (ZnO) is added to a twin screw compounder (Wrarner & Pfleiderer, Type ZSK 25) with respect to nylon resin. Mixing with h made the resin composition into chips. A zinc oxide (ZnO) -containing resin composition was added to the sheath and a nylon resin was added to the core. At this time, the ratio of S (second part) / C (deep part) was 5: 5. After inserting a spinneret having a spinneret having a number of 24 spinnerets, the spinning machine was spun at a spinning speed of 4000 m / min at a spinning temperature of 270 ° C., followed by stretching at a draw ratio of 2 to prepare 40 denier / 24 filament fibers. The cross section of the fiber shows a state in which zinc oxide nanoparticles are well dispersed in the projection electron micrograph of FIG. The fiber was photo-deposited by ultraviolet irradiation for 60 seconds while immersing in a solution consisting of an aqueous solution of silver nitrate (AgNO 3) and methanol at a concentration of 1.5 × 10 −4 mol. At the time of photodeposition, the distance from the light source was maintained at 5 cm, and the fiber (Ag) supported on the zinc oxide (ZnO) particles was washed with distilled water and dried at room temperature. FIG. 3 shows a photograph of the fiber on which the silver particles are photo-deposited, and as can be seen from the EDS analysis result of FIG. 4 and the XPS result of FIG. 5, the silver particles are supported.
[실시예 5 ]Example 5
나일론 (Nylon) 수지에 대해 1중량부의 50nm 사이즈의 산화아연(ZnO)을 트윈스크류 컴파운더(Wrarner & Pfleiderer , Type ZSK 25)에 투입하고 온도 260℃ 내지 290℃에서 스크류속도 250 rpm, 토출량 l5kg/h로 혼합하여 수지 조성물을 칩으로 만들었다. 산화아연(ZnO) 함유 수지 조성물을 초부(sheath)에 투입하고 나일론(Nylon) 수지를 심부(core)에 투입하였다. 이때 S(초부)/C(심부)의 비는 5:5로 하였다. 방사구멍 수가 24홀인 방사구금이 장착된 복합방사기에 투입한 다음 방사온도 270℃에서 권취속도 4000m/분으로 방사한 후, 연신비 2로 연신하여 40데니어/24필라멘트의 섬유를 제조하였다. 상기 섬유를 1.5×10-4 mol 농도의 질산은(AgNO3) 수용액과 메탄올로 이루어진 용액에 침지한 상태에서 120초 동안 자외선조사하여 광증착하였다. 광증착시 광원과의 거리를 5cm로 유지하고 상기 은(Ag)이 산화아연(ZnO) 입자상에 담지된 섬유를 증류수로 수세 후 상온 건조하였다. 도 3에서 은 입자가 광증착된 섬유의 사진을 보여주며, 도 4의 EDS 분석결과 및 도 5의XPS 결과에서 알 수 있듯이 은 입자가 담지되어 있음을 알 수 있다.
1 part by weight of 50 nm zinc oxide (ZnO) is added to a twin screw compounder (Wrarner & Pfleiderer, Type ZSK 25) with respect to nylon resin. Mixing with h made the resin composition into chips. A zinc oxide (ZnO) -containing resin composition was added to the sheath and a nylon resin was added to the core. At this time, the ratio of S (second part) / C (deep part) was 5: 5. After inserting a spinneret having a spinneret having a number of 24 spinnerets, the spinning machine was spun at a spinning speed of 4000 m / min at a spinning temperature of 270 ° C., followed by stretching at a draw ratio of 2 to prepare 40 denier / 24 filament fibers. The fiber was photodeposited by ultraviolet irradiation for 120 seconds while immersing in a solution consisting of an aqueous solution of silver nitrate (AgNO 3) and methanol at a concentration of 1.5 × 10 −4 mol. At the time of photodeposition, the distance from the light source was maintained at 5 cm, and the fiber (Ag) supported on the zinc oxide (ZnO) particles was washed with distilled water and dried at room temperature. FIG. 3 shows a photograph of the fiber on which the silver particles are photo-deposited, and as can be seen from the EDS analysis result of FIG. 4 and the XPS result of FIG. 5, it can be seen that silver particles are supported.
[실시예 6 ]Example 6
나일론 (Nylon) 수지에 대해 1중량부의 50nm 사이즈의 산화아연(ZnO)을 트윈스크류 컴파운더(Wrarner & Pfleiderer , Type ZSK 25)에 투입하고 온도 260℃ 내지 290℃에서 스크류속도 250 rpm, 토출량 l5kg/h로 혼합하여 수지 조성물을 칩으로 만들었다. 산화아연(ZnO) 함유 수지 조성물을 초부(sheath)에 투입하고 나일론(Nylon) 수지를 심부(core)에 투입하였다. 이때 S(초부)/C(심부)의 비는 5:5로 하였다. 방사구멍 수가 24홀인 방사구금이 장착된 복합방사기에 투입한 다음 방사온도 270℃에서 권취속도 4000m/분으로 방사한 후, 연신비 2로 연신하여 40데니어/24필라멘트의 섬유를 제조하였다. 상기 섬유를 1.5×10-4 mol 농도의 질산은(AgNO3) 수용액과 메탄올로 이루어진 용액에 침지한 상태에서 180초 동안 자외선조사하여 광증착하였다. 광증착시 광원과의 거리를 5cm로 유지하고 상기 은(Ag)이 산화아연(ZnO) 입자상에 담지된 섬유를 증류수로 수세 후 상온 건조하였다. 도 3에서 은 입자가 광증착된 섬유의 사진을 보여주며, 도 4의 EDS 분석결과 및 도 5의XPS 결과에서 알 수 있듯이 은 입자가 담지되어 있음을 알 수 있다.1 part by weight of 50 nm zinc oxide (ZnO) is added to a twin screw compounder (Wrarner & Pfleiderer, Type ZSK 25) with respect to nylon resin. Mixing with h made the resin composition into chips. A zinc oxide (ZnO) -containing resin composition was added to the sheath and a nylon resin was added to the core. At this time, the ratio of S (second part) / C (deep part) was 5: 5. After inserting a spinneret having a spinneret having a number of 24 spinnerets, the spinning machine was spun at a spinning speed of 4000 m / min at a spinning temperature of 270 ° C., followed by stretching at a draw ratio of 2 to prepare 40 denier / 24 filament fibers. The fiber was photodeposited by ultraviolet irradiation for 180 seconds while being immersed in a solution consisting of an aqueous solution of silver nitrate (AgNO 3) and methanol at a concentration of 1.5 × 10 −4 mol. At the time of photodeposition, the distance from the light source was maintained at 5 cm, and the fiber (Ag) supported on the zinc oxide (ZnO) particles was washed with distilled water and dried at room temperature. FIG. 3 shows a photograph of the fiber on which the silver particles are photo-deposited, and as can be seen from the EDS analysis result of FIG. 4 and the XPS result of FIG. 5, it can be seen that silver particles are supported.
상기 실시예 1, 2, 3, 4, 5, 6에서 얻어진 섬유를 제직한 직물의 항균성 및 자외선 차단성은 하기의 방법으로 측정하였다.The antimicrobial and ultraviolet ray blocking properties of the woven fabric of the fibers obtained in Examples 1, 2, 3, 4, 5, and 6 were measured by the following method.
- 항균성: KS K 0693 방법을 준용하였으며 공시균은 Staphylococcus aureus,Klebsiella pneumoniae을 시험균종으로 하였으며 정균 감소율로 나타내었다.Antimicrobial activity: KS K 0693 was used. The test strains were Staphylococcus aureus and Klebsiella pneumoniae.
- 자외선 차단성 평가실험은 KS K 0850(섬유제품의 자외선 차단율 및 차단 지수 시험방법)에 따라 평가하였으며 차단율은 하기의 식에 의해 계산하였다. 자외선-A(UV-A)는 파장이 315～400nm인 태양 자외선영역이며 자외선-B는 파장이 280～315nm인 태양 자외선영역이다. 자외선 실험은 샘플을 분광광도계의 샘플 홀드에 고정시킨 후 파장 290에서 400nm를 5nm 파장 단위로 주사하여 샘플의 자외선 투과율을 측정한다.-UV protection test was evaluated according to KS K 0850 (UV protection rate and blocking index test method of textile products) and the blocking rate was calculated by the following equation. UV-A (UV-A) is a solar ultraviolet region with a wavelength of 315-400 nm and UV-B is a solar ultraviolet region with a wavelength of 280-315 nm. In the ultraviolet experiment, the sample is fixed to the sample hold of the spectrophotometer, and then the wavelength of 290 to 400 nm is scanned in 5 nm wavelength units to measure the ultraviolet transmittance of the sample.
표 1은 본 발명의 실시예 예 1, 2, 3, 4, 5, 6의 복합섬유의 항균성 및 자외선 차단성을 평가한 결과를 나타낸 것이다. 하기 표 1에서 알 수 있는 바와 같이, 본 발명의 은이 광증착에 의해 담지된 섬의 항균성 및 자외선 차단능이 우수하다는 것을 알 수 있다. Table 1 shows the results of evaluating the antimicrobial and ultraviolet ray blocking properties of the composite fibers of Examples 1, 2, 3, 4, 5, and 6 of the present invention. As can be seen in Table 1, it can be seen that the silver of the present invention is excellent in the antimicrobial and ultraviolet blocking ability of the island supported by the light deposition.
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