KR100885428B1 - Conductive nylon fiber and method of preparing the same - Google Patents
Conductive nylon fiber and method of preparing the same Download PDFInfo
- Publication number
- KR100885428B1 KR100885428B1 KR1020080036544A KR20080036544A KR100885428B1 KR 100885428 B1 KR100885428 B1 KR 100885428B1 KR 1020080036544 A KR1020080036544 A KR 1020080036544A KR 20080036544 A KR20080036544 A KR 20080036544A KR 100885428 B1 KR100885428 B1 KR 100885428B1
- Authority
- KR
- South Korea
- Prior art keywords
- group
- silane
- fiber
- nylon fiber
- silane group
- Prior art date
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- 229920001778 nylon Polymers 0.000 title claims abstract description 123
- 238000000034 method Methods 0.000 title claims description 35
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical group [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims abstract description 127
- OMZSGWSJDCOLKM-UHFFFAOYSA-N copper(II) sulfide Chemical compound [S-2].[Cu+2] OMZSGWSJDCOLKM-UHFFFAOYSA-N 0.000 claims abstract description 62
- 239000007864 aqueous solution Substances 0.000 claims abstract description 40
- 229910000077 silane Inorganic materials 0.000 claims abstract description 30
- 238000004519 manufacturing process Methods 0.000 claims abstract description 22
- NLHHRLWOUZZQLW-UHFFFAOYSA-N Acrylonitrile Chemical compound C=CC#N NLHHRLWOUZZQLW-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000000835 fiber Substances 0.000 claims description 88
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 claims description 30
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 22
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 21
- 229910052751 metal Inorganic materials 0.000 claims description 16
- 239000002184 metal Substances 0.000 claims description 16
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 15
- 235000010265 sodium sulphite Nutrition 0.000 claims description 15
- 239000000243 solution Substances 0.000 claims description 14
- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical class [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 claims description 10
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 10
- 239000002253 acid Substances 0.000 claims description 9
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 claims description 9
- 229910000366 copper(II) sulfate Inorganic materials 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 8
- AKHNMLFCWUSKQB-UHFFFAOYSA-L sodium thiosulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=S AKHNMLFCWUSKQB-UHFFFAOYSA-L 0.000 claims description 8
- 235000019345 sodium thiosulphate Nutrition 0.000 claims description 8
- 239000003638 chemical reducing agent Substances 0.000 claims description 7
- 239000003002 pH adjusting agent Substances 0.000 claims description 7
- 150000003464 sulfur compounds Chemical class 0.000 claims description 7
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 6
- 239000000706 filtrate Substances 0.000 claims description 6
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims description 6
- 239000012966 redox initiator Substances 0.000 claims description 6
- 239000001488 sodium phosphate Substances 0.000 claims description 6
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 claims description 5
- 239000001632 sodium acetate Substances 0.000 claims description 5
- 235000017281 sodium acetate Nutrition 0.000 claims description 5
- KWSLGOVYXMQPPX-UHFFFAOYSA-N 5-[3-(trifluoromethyl)phenyl]-2h-tetrazole Chemical compound FC(F)(F)C1=CC=CC(C2=NNN=N2)=C1 KWSLGOVYXMQPPX-UHFFFAOYSA-N 0.000 claims description 4
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 4
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 4
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 4
- RAHZWNYVWXNFOC-UHFFFAOYSA-N Sulphur dioxide Chemical compound O=S=O RAHZWNYVWXNFOC-UHFFFAOYSA-N 0.000 claims description 4
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 claims description 4
- OPQARKPSCNTWTJ-UHFFFAOYSA-L copper(ii) acetate Chemical compound [Cu+2].CC([O-])=O.CC([O-])=O OPQARKPSCNTWTJ-UHFFFAOYSA-L 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 4
- FWDBOZPQNFPOLF-UHFFFAOYSA-N ethenyl(triethoxy)silane Chemical compound CCO[Si](OCC)(OCC)C=C FWDBOZPQNFPOLF-UHFFFAOYSA-N 0.000 claims description 4
- NKSJNEHGWDZZQF-UHFFFAOYSA-N ethenyl(trimethoxy)silane Chemical compound CO[Si](OC)(OC)C=C NKSJNEHGWDZZQF-UHFFFAOYSA-N 0.000 claims description 4
- HYBBIBNJHNGZAN-UHFFFAOYSA-N furfural Chemical compound O=CC1=CC=CO1 HYBBIBNJHNGZAN-UHFFFAOYSA-N 0.000 claims description 4
- 229910001379 sodium hypophosphite Inorganic materials 0.000 claims description 4
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 3
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 claims description 3
- 239000010949 copper Substances 0.000 claims description 3
- 229910052802 copper Inorganic materials 0.000 claims description 3
- BNIILDVGGAEEIG-UHFFFAOYSA-L disodium hydrogen phosphate Chemical compound [Na+].[Na+].OP([O-])([O-])=O BNIILDVGGAEEIG-UHFFFAOYSA-L 0.000 claims description 3
- 229910000397 disodium phosphate Inorganic materials 0.000 claims description 3
- 235000019800 disodium phosphate Nutrition 0.000 claims description 3
- 229910000037 hydrogen sulfide Inorganic materials 0.000 claims description 3
- 229910000162 sodium phosphate Inorganic materials 0.000 claims description 3
- 235000011008 sodium phosphates Nutrition 0.000 claims description 3
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 claims description 3
- LCPVQAHEFVXVKT-UHFFFAOYSA-N 2-(2,4-difluorophenoxy)pyridin-3-amine Chemical compound NC1=CC=CN=C1OC1=CC=C(F)C=C1F LCPVQAHEFVXVKT-UHFFFAOYSA-N 0.000 claims description 2
- YIVJZNGAASQVEM-UHFFFAOYSA-N Lauroyl peroxide Chemical compound CCCCCCCCCCCC(=O)OOC(=O)CCCCCCCCCCC YIVJZNGAASQVEM-UHFFFAOYSA-N 0.000 claims description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 2
- LSNNMFCWUKXFEE-UHFFFAOYSA-N Sulfurous acid Chemical compound OS(O)=O LSNNMFCWUKXFEE-UHFFFAOYSA-N 0.000 claims description 2
- 230000002378 acidificating effect Effects 0.000 claims description 2
- 239000003513 alkali Substances 0.000 claims description 2
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium peroxydisulfate Substances [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 2
- VAZSKTXWXKYQJF-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)OOS([O-])=O VAZSKTXWXKYQJF-UHFFFAOYSA-N 0.000 claims description 2
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 2
- UNTBPXHCXVWYOI-UHFFFAOYSA-O azanium;oxido(dioxo)vanadium Chemical compound [NH4+].[O-][V](=O)=O UNTBPXHCXVWYOI-UHFFFAOYSA-O 0.000 claims description 2
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 2
- 235000010216 calcium carbonate Nutrition 0.000 claims description 2
- 229940076286 cupric acetate Drugs 0.000 claims description 2
- 229960003280 cupric chloride Drugs 0.000 claims description 2
- 239000011790 ferrous sulphate Substances 0.000 claims description 2
- 235000003891 ferrous sulphate Nutrition 0.000 claims description 2
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 claims description 2
- 229910000359 iron(II) sulfate Inorganic materials 0.000 claims description 2
- 229910017604 nitric acid Inorganic materials 0.000 claims description 2
- JRKICGRDRMAZLK-UHFFFAOYSA-L peroxydisulfate Chemical compound [O-]S(=O)(=O)OOS([O-])(=O)=O JRKICGRDRMAZLK-UHFFFAOYSA-L 0.000 claims description 2
- 150000003839 salts Chemical class 0.000 claims description 2
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 2
- 235000017550 sodium carbonate Nutrition 0.000 claims description 2
- HRZFUMHJMZEROT-UHFFFAOYSA-L sodium disulfite Chemical compound [Na+].[Na+].[O-]S(=O)S([O-])(=O)=O HRZFUMHJMZEROT-UHFFFAOYSA-L 0.000 claims description 2
- 235000011121 sodium hydroxide Nutrition 0.000 claims description 2
- 235000010262 sodium metabisulphite Nutrition 0.000 claims description 2
- CHQMHPLRPQMAMX-UHFFFAOYSA-L sodium persulfate Substances [Na+].[Na+].[O-]S(=O)(=O)OOS([O-])(=O)=O CHQMHPLRPQMAMX-UHFFFAOYSA-L 0.000 claims description 2
- 229910052979 sodium sulfide Inorganic materials 0.000 claims description 2
- GRVFOGOEDUUMBP-UHFFFAOYSA-N sodium sulfide (anhydrous) Chemical compound [Na+].[Na+].[S-2] GRVFOGOEDUUMBP-UHFFFAOYSA-N 0.000 claims description 2
- 235000010269 sulphur dioxide Nutrition 0.000 claims description 2
- 238000005406 washing Methods 0.000 abstract description 20
- 230000006866 deterioration Effects 0.000 abstract description 2
- 239000004753 textile Substances 0.000 abstract 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 23
- 239000004677 Nylon Substances 0.000 description 19
- 238000006243 chemical reaction Methods 0.000 description 16
- 230000008569 process Effects 0.000 description 14
- 240000007817 Olea europaea Species 0.000 description 11
- 238000004458 analytical method Methods 0.000 description 9
- 239000000843 powder Substances 0.000 description 8
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 description 6
- -1 palladium ions Chemical class 0.000 description 6
- 238000007747 plating Methods 0.000 description 5
- 238000001179 sorption measurement Methods 0.000 description 5
- 239000006229 carbon black Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000009987 spinning Methods 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 230000008859 change Effects 0.000 description 3
- 230000005611 electricity Effects 0.000 description 3
- MASNVFNHVJIXLL-UHFFFAOYSA-N ethenyl(ethoxy)silicon Chemical compound CCO[Si]C=C MASNVFNHVJIXLL-UHFFFAOYSA-N 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 230000000704 physical effect Effects 0.000 description 3
- 239000011148 porous material Substances 0.000 description 3
- BYOIQYHAYWYSCZ-UHFFFAOYSA-N prop-2-enoxysilane Chemical compound [SiH3]OCC=C BYOIQYHAYWYSCZ-UHFFFAOYSA-N 0.000 description 3
- 230000003068 static effect Effects 0.000 description 3
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 3
- 229920002972 Acrylic fiber Polymers 0.000 description 2
- 239000002216 antistatic agent Substances 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 238000006664 bond formation reaction Methods 0.000 description 2
- 229910001431 copper ion Inorganic materials 0.000 description 2
- 238000000151 deposition Methods 0.000 description 2
- 238000007772 electroless plating Methods 0.000 description 2
- 239000003446 ligand Substances 0.000 description 2
- PHQOGHDTIVQXHL-UHFFFAOYSA-N n'-(3-trimethoxysilylpropyl)ethane-1,2-diamine Chemical compound CO[Si](OC)(OC)CCCNCCN PHQOGHDTIVQXHL-UHFFFAOYSA-N 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- XFXPMWWXUTWYJX-UHFFFAOYSA-N Cyanide Chemical compound N#[C-] XFXPMWWXUTWYJX-UHFFFAOYSA-N 0.000 description 1
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 description 1
- 238000001994 activation Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 230000009918 complex formation Effects 0.000 description 1
- 229910000365 copper sulfate Inorganic materials 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000002845 discoloration Methods 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- 238000002149 energy-dispersive X-ray emission spectroscopy Methods 0.000 description 1
- 238000007380 fibre production Methods 0.000 description 1
- 238000010559 graft polymerization reaction Methods 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 150000002825 nitriles Chemical group 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- KDLHZDBZIXYQEI-UHFFFAOYSA-N palladium Substances [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 1
- NFIYTPYOYDDLGO-UHFFFAOYSA-N phosphoric acid;sodium Chemical compound [Na].OP(O)(O)=O NFIYTPYOYDDLGO-UHFFFAOYSA-N 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- OTYBMLCTZGSZBG-UHFFFAOYSA-L potassium sulfate Chemical compound [K+].[K+].[O-]S([O-])(=O)=O OTYBMLCTZGSZBG-UHFFFAOYSA-L 0.000 description 1
- 229910052939 potassium sulfate Inorganic materials 0.000 description 1
- 235000011151 potassium sulphates Nutrition 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 239000012266 salt solution Substances 0.000 description 1
- 230000001235 sensitizing effect Effects 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
- 239000011550 stock solution Substances 0.000 description 1
- 229920002994 synthetic fiber Polymers 0.000 description 1
- 239000012209 synthetic fiber Substances 0.000 description 1
- YUYCVXFAYWRXLS-UHFFFAOYSA-N trimethoxysilane Chemical compound CO[SiH](OC)OC YUYCVXFAYWRXLS-UHFFFAOYSA-N 0.000 description 1
- UKRDPEFKFJNXQM-UHFFFAOYSA-N vinylsilane Chemical group [SiH3]C=C UKRDPEFKFJNXQM-UHFFFAOYSA-N 0.000 description 1
- 230000037303 wrinkles Effects 0.000 description 1
Classifications
-
- 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
- D06M11/45—Oxides or hydroxides of elements of Groups 3 or 13 of the Periodic Table; Aluminates
-
- 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
- D06M11/77—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 silicon or compounds thereof
-
- 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
- D06M11/83—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 metals; with metal-generating compounds, e.g. metal carbonyls; Reduction of metal compounds on textiles
-
- 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
- D06M13/244—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 sulfur or phosphorus
-
- 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
- D06M13/322—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 nitrogen
- D06M13/345—Nitriles
- D06M13/348—Nitriles unsaturated, e.g. acrylonitrile
-
- 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
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/16—Synthetic fibres, other than mineral fibres
- D06M2101/30—Synthetic polymers consisting of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M2101/34—Polyamides
-
- 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
- D10B2331/00—Fibres made from polymers obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. polycondensation products
- D10B2331/02—Fibres made from polymers obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. polycondensation products polyamides
-
- 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
- D10B2401/16—Physical properties antistatic; conductive
Landscapes
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
- Chemical Or Physical Treatment Of Fibers (AREA)
Abstract
Description
본 발명은 도전성 나일론 섬유 및 그 제조방법에 관한 것으로서, 보다 구체적으로는 우수한 도전성과 내세탁 특성이 우수한 도전성 나일론 섬유 및 그 제조방법에 관한 것이다.The present invention relates to a conductive nylon fiber and a method for producing the same, and more particularly, to a conductive nylon fiber and an excellent method for producing excellent conductive and laundry resistance.
대부분의 합성섬유와 일부 천연섬유는 섬유간의 마찰이나, 섬유와 피부간의 마찰에 의하여 정전기가 발생되어 대전됨은 이미 알려진 사실로, 이러한 정전기 발생은 피복의 착용에서 뿐만 아니라 산업 현장에서도 큰 문제를 발생시키는 것으로 알려져 있다.It is known that most synthetic fibers and some natural fibers are charged by static electricity due to friction between fibers or friction between fibers and skin. This generation of static electricity is a major problem not only in the wearing of the coating but also in the industrial field. It is known.
이러한 섬유의 정전기 발생문제를 해소하기 위하여 후처리 공정에서 대전 방지제 처리를 하거나, 섬유자체에 도전성을 부여하는 방법 등이 개발되고 있다.In order to solve the static electricity generation problem of the fiber, a method for treating the antistatic agent in the post-treatment process, or imparting conductivity to the fiber itself has been developed.
대전 방지제를 이용하여 섬유를 처리하는 경우에는 값싸고 공정이 간단한 장점이 있으나, 세탁 및 장시간 사용 시 대전 방지 효과가 없어지는 단점이 있다.When the fiber is treated using an antistatic agent, there is an advantage that the process is inexpensive and simple, but there is a disadvantage that the antistatic effect is lost when washing and using for a long time.
또한, 섬유자체에 도전성을 부여하는 방법으로는 도전성을 가지는 카본블랙 이나 금속 분말을 중합체에 혼합 및 반죽하여 방사원액을 만든 다음, 가는 구금을 통과 시켜 섬유화하는 방법과 섬유 표면에 금속을 도금하는 방법, 섬유 표면에 존재하는 구멍에 금속 분말을 침착시키는 방법 등이 있다. In addition, as a method of imparting conductivity to the fiber itself, carbon black or metal powder having conductivity is mixed and kneaded in a polymer to form a spinning stock solution, and then passed through a thin mold to form a fiber and a method of plating a metal on the surface of the fiber. And a method of depositing a metal powder in a hole present on a fiber surface.
카본블랙이나 금속 분말을 중합체에 혼합, 방사하여 도전성 섬유를 만드는 방법의 경우에는 도전성을 띄는 카본블랙이나 금속 분말이 방사구금을 통과하여 섬유화되는 과정에서 방사에 영향을 미치지 않을 정도로 작은 입자(예를 들면 나노입자)이어야 한다. 그러나, 상기와 같은 나노입자는 굉장히 고가이며, 원하는 만큼의 도전성을 얻기 위해서는 많은 양의 카본블랙이나 금속 분말을 섬유에 혼합하여야 하기 때문에 경제성을 확보하기 어렵다. 특히, 다량의 카본블랙을 섬유에 혼합할 경우에는 섬유 자체의 물성, 즉 섬유의 강도, 신도 및 방사성 등이 크게 저하될 뿐 아니라, 섬유 전체가 흑색을 띄게 되어 섬유의 외관을 손상시키는 단점이 있다.In the case of mixing carbon black or metal powder into a polymer to form conductive fibers, particles which are small enough to have no effect on spinning in the process of forming the conductive carbon black or metal powder through the spinneret and being fiberized For example nanoparticles). However, such nanoparticles are very expensive, and in order to obtain the desired conductivity, it is difficult to secure economic feasibility because a large amount of carbon black or metal powder must be mixed with the fibers. In particular, when a large amount of carbon black is mixed with the fiber, the physical properties of the fiber itself, that is, the strength, elongation, and radioactivity of the fiber, are greatly reduced, and the entire fiber becomes black, which impairs the appearance of the fiber. .
섬유 표면을 금속으로 도금하여 도전성을 부여할 경우 대부분 무전해 도금법을 이용하여 처리하는 데, 이 때 섬유와 금속 도금간의 밀착성을 양호하게 하기 위해서는 미리 섬유표면에 주름을 형성시켜 주는 공정, 강산을 사용한 센시티빙 공정, 팔라듐 이온을 사용한 활성화 공정 등이 필요하다. 따라서, 무전해 도금액에 담궈 금속을 섬유 표면에 도금하는 공정 등의 공정이 복잡하고, 고도의 도금 기술을 필요로 한다. 또한, 이렇게 얻어진 도전성 섬유는 섬유 본래의 물성을 기대하기 어려울 뿐 아니라 내세탁성이 매우 낮은 단점이 있다. In the case of imparting conductivity by plating the surface of the metal with metal, most of them are treated using electroless plating. In this case, in order to improve the adhesion between the fiber and the metal plating, wrinkles are formed on the surface of the fiber beforehand. A sensitizing process, an activation process using palladium ions, and the like are required. Therefore, processes, such as a process of plating a metal on a fiber surface by immersing in an electroless plating liquid, are complicated and require a high plating technique. In addition, the conductive fiber thus obtained is not only difficult to expect the inherent physical properties of the fiber, but also has the disadvantage of having very low washing resistance.
섬유 표면에 존재하는 구멍에 금속 분말을 침착시키는 방법은 도전성을 지닌 금속 분말의 입자보다 큰 구멍이 섬유에 있어야 하는 데 일반적인 방사법으로 제조 되는 섬유의 경우 금속 분말을 침착시키기에는 구멍의 크기가 금속 분말의 입자보다 훨씬 적어 불가능하다. 이를 위해서는 섬유 제조 시 특별히 다공성의 섬유를 제조하여야만 한다. 다공성 섬유의 제조는 독특한 방사법이 요구될 뿐 만 아니라, 다양한 규격의 섬유를 제조함에 한계가 있어 실생활에의 적용에 제약이 따른다.The method of depositing the metal powder in the pores present on the surface of the fiber requires that the fiber has pores larger than the particles of the conductive metal powder. In the case of fibers manufactured by the conventional spinning method, the size of the pores is not sufficient to deposit the metal powder. Much less than the particles of is impossible. For this purpose, a particularly porous fiber must be prepared during the fiber production. The production of porous fibers not only requires a unique spinning method, but also has limitations in the production of fibers of various specifications, thus limiting their application to real life.
따라서 상기의 방법과 같은 가공상의 어려움을 해소하고 원하는 내세탁성을 가지는 도전성 섬유의 개발이 수행되어 왔으며, 특히 아크릴 섬유에 도전성이 우수한 황화구리를 함유시키는 방법이 한국 특허공고 제1984-0002109호, 한국 특허공고 제1987-0001339호, 한국 특허공고 제1987-0000745호, 및 한국 특허공고 제1996-011594호에 의하여 제안된 바 있다.Therefore, the development of conductive fibers having the desired washing resistance and the processing difficulties such as the above method has been carried out. Particularly, a method of containing copper sulfide having excellent conductivity in acrylic fibers is disclosed in Korean Patent Publication No. 1984-0002109, Korean Patent Publication No. 1987-0001339, Korean Patent Publication No. 1987-0000745, and Korean Patent Publication No. 1996-011594.
상기의 발명들은 아크릴 섬유의 시안기와 2가 구리이온으로부터 얻어진 황화구리간의 배위결합에 의해 착물을 형성하여 도전성이 우수한 섬유를 제조하고자 하였다. 하지만 나일론 섬유에 상기 방법을 적용할 경우 섬유 자체에 2가 구리 수용액으로부터 환원된 1가 구리이온과 착물을 형성할 수 있는 리간드가 존재하지 않아 도전성이 우수한 황화구리를 도입할 수가 없었다.The inventions described above are intended to produce a fiber having excellent conductivity by forming a complex by the coordinating bond between the cyan group of the acrylic fiber and copper sulfide obtained from divalent copper ions. However, when the above method was applied to nylon fibers, there was no ligand capable of forming a complex with monovalent copper ions reduced from a divalent copper aqueous solution, and thus copper sulfide having excellent conductivity could not be introduced.
이러한 문제점을 극복하기 위한 노력이 이루어져 왔으며, 미국특허 제3,940,553호에는 나일론 섬유를 처음에 황화수소와 접촉시키고, 황화수소가 도입된 섬유를 황산구리 수용액 등의 금속염 용액에 적심으로써 섬유상에 황화구리 등의 황화금속의 부착물이 형성되도록 하는, 나일론 섬유에 전기 전도성을 부여하는 방법이 제안되어 있다. 하지만, 이 방법에 의하여 얻어진 섬유상의 황화구리 부착물은 안정성이 떨어지고, 특히 세정성이 매우 낮아 사용도중에 전기 전도성이 서서히 감소되는 문제가 있다.Efforts have been made to overcome these problems, and US Patent No. 3,940,553 discloses that nylon fibers are first contacted with hydrogen sulfide, and the hydrogen sulfide-introduced fibers are immersed in a metal salt solution such as copper sulfate aqueous solution. A method of imparting electrical conductivity to nylon fibers has been proposed that allows the formation of deposits of. However, the fibrous copper sulfide deposit obtained by this method is inferior in stability, and in particular, the cleaning property is very low so that the electrical conductivity gradually decreases during use.
또한, 미국특허 4,378,226호에는 나일론 섬유에 아크릴로니트릴을 그라프트 중합시켜 시안기를 갖는 섬유와 이 섬유에 결합된 황화구리를 포함하는 전기전도성 섬유가 기재되어 있다. 상기 방법에 의한 전도성 섬유는 우수한 전기 전도성과 개량된 세정성을 나타내지만, 섬유에 시안기를 도입시키기 위한 그라프트 중합공정이 매우 까다롭고, 섬유의 표면 뿐만 아니라 그 내부까지 중합이 진행됨에 따라 도전성 섬유의 두께가 증가하고 섬유의 물리적 성질이 변하는 결점이 있다.U.S. Patent No. 4,378,226 also discloses an electrically conductive fiber comprising graft polymerized acrylonitrile on nylon fibers having a cyan group and copper sulfide bonded to the fibers. The conductive fiber by the above method exhibits excellent electrical conductivity and improved detergency, but the graft polymerization process for introducing cyan groups into the fiber is very difficult, and as the polymerization proceeds not only to the surface of the fiber but also to the inside thereof, the conductive fiber There is a drawback of increasing the thickness of and changing the physical properties of the fibers.
본 발명은 상기와 같은 문제점을 해결하기 위한 것으로서, 본 발명의 목적은 황화구리와 강한 결합 또는 황화구리를 흡착할 수 있는 실란기를 섬유 표면에 도입하여 우수한 도전성과 내세탁 특성을 가지는 도전성 나일론 섬유 및 그 제조방법을 제공하는 것이다.The present invention is to solve the above problems, an object of the present invention is to introduce a conductive nylon fiber having excellent conductivity and washing resistance by introducing a silane group capable of adsorbing a copper sulfide and a strong bond or copper sulfide to the fiber surface and It is to provide a manufacturing method.
본 발명의 또 다른 목적은, 섬유 표면에 도입된 실란기에 도전성이 우수한 황화구리와 배위결합에 의한 착물을 형성할 수 있는 시안기를 추가로 형성하는 도전성 나일론 섬유 및 그 제조방법을 제공하는 것이다.It is still another object of the present invention to provide a conductive nylon fiber which further forms a cyan group capable of forming a complex by coordination bond with copper sulfide having excellent conductivity, and a method for producing the silane group introduced on the fiber surface.
본 발명은 상기 목적을 달성하기 위하여, 섬유 표면에 실란기 및 상기 실란기에 흡착 또는 배위결합되는 황화구리를 포함하는 것인, 도전성 나일론 섬유를 제공한다.The present invention provides a conductive nylon fiber, which comprises a copper sulfide adsorbed or coordinated to the silane group and the silane group on the fiber surface to achieve the above object.
상기 도전성 나일론 섬유의 제조방법은, (a) 나일론 섬유에 실란기를 도입하여 실란기 함유 나일론 섬유를 제조하는 단계; 및 (b) 상기 실란기 함유 나일론 섬유에 황화구리를 흡착 또는 배위결합시키는 단계를 포함한다.The method for producing a conductive nylon fiber, (a) introducing a silane group to the nylon fiber to produce a silane group-containing nylon fiber; And (b) adsorbing or coordinating copper sulfide to the silane group-containing nylon fiber.
또한, 본 발명의 또 다른 일실시예에 따르면, 섬유 표면에 실란기, 시안기 및 상기 실란기와 시안기에 흡착 또는 배위결합되는 황화구리를 포함하는 것인, 도전성 나일론 섬유를 제공한다.In addition, according to another embodiment of the present invention, to provide a conductive nylon fiber, which comprises a copper sulfide adsorbed or coordinated to the silane group, cyan group and the silane group and cyan group on the fiber surface.
상기 도전성 나일론 섬유의 제조방법은, (a) 나일론 섬유에 실란기를 도입하여 실란기 함유 나일론 섬유를 제조하는 단계; (b) 상기 실란기 함유 나일론 섬유에 시안기를 도입하여 실란기 및 시안기 함유 나일론 섬유를 제조하는 단계; 및 (c) 상기 실란기 및 시안기 함유 나일론 섬유에 황화구리를 흡착 또는 배위결합시키는 단계를 포함한다.The method for producing a conductive nylon fiber, (a) introducing a silane group to the nylon fiber to produce a silane group-containing nylon fiber; (b) preparing a silane group and a cyan group-containing nylon fiber by introducing a cyan group into the silane group-containing nylon fiber; And (c) adsorbing or coordinating copper sulfide to the silane group and the cyan group-containing nylon fiber.
이하, 본 발명을 보다 상세하게 설명한다.Hereinafter, the present invention will be described in more detail.
본 발명은 우수한 도전성을 가지는 황화구리를 흡착하거나 또는 강한 배위결합에 의해 착물을 형성할 수 있는 특정 리간드를 섬유 표면에 도입한 것을 특징으로 한다. 즉, 본 발명은 나일론 섬유 표면에 간단한 화학 반응으로 실란기를 도입하여 황화구리를 흡착하거나 더욱 강력한 배위결합을 형성하도록 한다. 또한, 본 발명은 상기 실란기가 도입된 나일론 섬유 표면에 아크릴로니트릴을 이용하여 간단한 화학반응을 진행시켜 시안기를 추가로 도입할 수 있고, 이들 역시 황화구리와 강한 흡착 또는 배위결합에 의한 착물이 형성되도록 한다. 따라서, 본 발명의 나일론 섬유는 잦은 세탁에도 그 결합을 유지하고, 황화구리의 이탈에 의한 변색 및 도전성의 저하를 방지할 수 있다.The present invention is characterized in that a specific ligand capable of adsorbing copper sulfide having excellent conductivity or forming a complex by strong coordination bonds is introduced into the fiber surface. That is, the present invention introduces a silane group to the surface of the nylon fiber by a simple chemical reaction to adsorb copper sulfide or to form a stronger coordination bond. In addition, the present invention can further introduce a cyan group by advancing a simple chemical reaction using acrylonitrile on the surface of the nylon fiber in which the silane group is introduced, and these also form a complex by copper sulfide and strong adsorption or coordination bond Be sure to Therefore, the nylon fiber of the present invention can maintain its bonding even after frequent washing, and can prevent discoloration and deterioration of conductivity due to detachment of copper sulfide.
이러한 본 발명의 바람직한 제1실시예에 따른 도전성 나일론 섬유는 섬유 표면에 실란기 및 상기 실란기에 흡착되거나 배위결합되는 황화구리를 포함한다.The conductive nylon fiber according to the first preferred embodiment of the present invention includes a silane group on the surface of the fiber and copper sulfide adsorbed or coordinated to the silane group.
본 발명의 제1실시예의 도전성 나일론 섬유의 표면에 도입되는 실란기는 섬유 전체 중량에 대해 각각 0.1 내지 5 중량%인 것이 충분한 도전성 및 내세탁 특성 을 향상시킴과 동시에 경제성 및 섬유의 기계적 물성 확보의 측면에서 바람직하고, 0.5 내지 2 중량%인 것이 더 바람직하다.The silane group introduced to the surface of the conductive nylon fiber of the first embodiment of the present invention is 0.1 to 5% by weight relative to the total weight of the fiber is sufficient to improve the conductivity and washing resistance, while at the same time improving the economical and mechanical properties of the fiber Is preferred, and more preferably 0.5 to 2% by weight.
또한, 상기 제1실시예의 도전성 섬유의 실란기에 배위결합되는 황화구리는 전체 섬유 중량에 대하여 1 내지 15 중량%로 포함하는 것이 충분한 도전성 및 기계적 물성 확보의 측면에서 바람직하다.In addition, copper sulfide coordinated to the silane group of the conductive fiber of the first embodiment is preferably included in an amount of 1 to 15% by weight based on the total fiber weight in terms of ensuring sufficient conductivity and mechanical properties.
상기 제1실시예에 따른 도전성 나일론 섬유의 제조방법은 나일론 섬유 표면에 실란기를 도입하여 실란기 함유 나일론 섬유를 제조하고, 상기 실란기 함유 나일론 섬유에 황화구리를 흡착하거나 배위결합을 형성시키는 단계를 포함할 수 있다.The method of manufacturing a conductive nylon fiber according to the first embodiment is a step of preparing a silane group-containing nylon fiber by introducing a silane group on the surface of the nylon fiber, adsorbing copper sulfide or forming coordination bond on the silane group-containing nylon fiber It may include.
바람직하게, 상기 제1실시예의 도전성 나일론 섬유의 제조방법은Preferably, the manufacturing method of the conductive nylon fiber of the first embodiment
(a) 실란화합물 5 내지 25 g/L, 및 산 0.1 내지 10 g/L를 포함하는 실란 수용액을 이용하여 나일론 섬유에 실란기를 도입하여 실란기 함유 나일론 섬유를 제조하는 단계; 및(a) preparing a silane group-containing nylon fiber by introducing a silane group into the nylon fiber using an silane solution containing 5 to 25 g / L of silane compound and 0.1 to 10 g / L of acid; And
(b) 구리 이온염 2.5 내지 50 g/L, 환원제 0.5 내지 20 g/L, 황화합물 1 내지 30 g/L, 및 pH 조절제 5 내지 45 g/L를 포함하는 황화구리 수용액을 이용하여 상기 실란기 함유 나일론 섬유에 황화구리를 흡착 또는 배위결합시키는 단계를 순차적으로 진행하여 이루어질 수 있다.(b) the silane group using a copper sulfide aqueous solution containing 2.5 to 50 g / L of copper ion salt, 0.5 to 20 g / L of reducing agent, 1 to 30 g / L of sulfur compound, and 5 to 45 g / L of pH adjusting agent. Adsorption or coordination of the copper sulfide to the containing nylon fibers may be carried out sequentially.
상기 (a)단계는 i) 상기 실란 수용액 중에서 나일론 섬유를 30 내지 80 ℃로 0.1 내지 2시간 동안, 바람직하게 40 내지 60℃로 10분 내지 30분 동안 침지 후 여액의 실란 수용액을 제거하고 100 ℃로 유지시킨 건조기에 넣어 1 내지 2시간 건조 하거나, ii) 상기 실란 수용액 중에서 나일론 섬유를 40 내지 80 ℃로 1 내지 48시간 동안 반응을 진행시키는 것이 바람직하다Step (a) is i) immersed nylon fibers in the silane solution at 30 to 80 ℃ for 0.1 to 2 hours, preferably 10 minutes to 30 minutes at 40 to 60 ℃ remove the silane solution of the filtrate and 100 ℃ It is preferable to put in a drier maintained for 1 to 2 hours, or ii) to proceed the reaction in the silane aqueous solution at 40 to 80 ℃ for 1 to 48 hours.
또한, 상기 (b)단계는 반응 효율 및 공정 시간 단축의 측면을 고려하여, 상기 황화구리 수용액 중에서 실란기 함유 나일론 섬유를 40 내지 90 ℃로 1 내지 24시간 동안 반응을 진행시키는 것이 바람직하다.In addition, in the step (b), it is preferable to proceed with the reaction of the silane group-containing nylon fiber at 40 to 90 ° C. for 1 to 24 hours in the copper sulfide aqueous solution in consideration of aspects of reaction efficiency and process time shortening.
이때, 상기 각 단계에서 사용되는 원료물질의 함량은 최적의 효과를 나타내기 위한 함량 범위를 한정한 것이므로, 상기 범위를 만족시키는 것이 실란기의 도입 및 황화구리의 흡착 또는 배위결합 형성 측면에서 바람직하나, 본 발명이 반드시 상기 범위로만 한정되는 것은 아니다.At this time, since the content of the raw material used in each step is limited to the content range for showing the optimum effect, it is preferable to satisfy the above range in terms of introduction of the silane group and adsorption or coordination bond formation of copper sulfide. However, the present invention is not necessarily limited to the above range.
또한, 본 발명의 바람직한 제2실시예에 따른 도전성 나일론 섬유는 추가로 시안기를 포함하여, 섬유 표면에 실란기 및 시안기와 이들에 흡착되거나 배위결합되는 황화구리를 포함한다.In addition, the conductive nylon fiber according to the second preferred embodiment of the present invention further includes a cyan group, and copper sulfide adsorbed or coordinated to the silane group and the cyan group on the fiber surface.
제2실시예의 도전성 나일론 섬유의 표면에 도입되는 실란기 및 시안기의 함량의 경우도 섬유 전체 중량에 대해 각각 0.1 내지 5 중량%인 것이 충분한 도전성 및 내세탁 특성을 향상시킴과 동시에 경제성 및 섬유의 기계적 물성 확보의 측면에서 바람직하고, 0.5 내지 2 중량%인 것이 더 바람직하다.In the case of the content of the silane group and the cyan group introduced to the surface of the conductive nylon fiber of the second embodiment, 0.1 to 5% by weight relative to the total weight of the fiber, respectively, is sufficient to improve the conductivity and washing resistance, It is preferable in terms of securing mechanical properties, and more preferably 0.5 to 2% by weight.
상기 제2실시예의 실란기 및 시안기에 배위결합되는 황화구리의 함량 또한 전체 섬유 중량에 대하여 1 내지 15 중량%로 포함하는 것이 충분한 도전성 및 기계적 물성 확보의 측면에서 바람직하다.The content of copper sulfide coordinated to the silane group and the cyan group of the second embodiment is also preferably included in an amount of 1 to 15% by weight based on the total fiber weight in terms of securing sufficient conductivity and mechanical properties.
또한, 상기 제2실시예에 따른 도전성 나일론 섬유의 제조방법은 나일론 섬유 표면에 비닐기가 포함되어 있는 실란화합물과 반응시켜 실란기를 도입하여 실란기 함유 나일론 섬유를 제조하고, 상기 실란기 함유 나일론 섬유에 아크릴로니트릴과 화학 반응을 통해 시안기를 도입하여 실란기 및 시안기 함유 나일론 섬유를 제조하고, 상기 실란기와 시안기가 도입된 섬유에 황화구리를 흡착하거나 배위결합을 형성시키는 단계를 포함할 수 있다.In addition, the method for producing a conductive nylon fiber according to the second embodiment is to react with a silane compound containing a vinyl group on the surface of the nylon fiber to introduce a silane group to produce a silane group-containing nylon fiber, to the silane group-containing nylon fiber It may include the step of introducing a cyan group through a chemical reaction with acrylonitrile to produce a silane group and a cyan group-containing nylon fibers, and adsorbing copper sulfide or forming a coordination bond to the fiber introduced with the silane group and the cyan group.
이때, 상기 실란기 및 시안기 함유 나일론 섬유의 제조단계는 나일론 섬유에 실란기를 도입후 순차적으로 시안기를 도입하여 이루어지거나, 나일론 섬유에 실란기 및 시안기를 동시에 도입하여 이루어질 수 있다.In this case, the production of the silane group and the cyan group-containing nylon fiber may be made by introducing a silane group to the nylon fiber after the introduction of the cyan group sequentially, or by introducing a silane group and a cyan group to the nylon fiber at the same time.
바람직하게, 상기 제2실시예의 도전성 나일론 섬유의 제조방법에 있어서, 나일론 섬유에 실란기 및 시안기를 순차적으로 도입하는 경우,Preferably, in the method for producing the conductive nylon fiber of the second embodiment, when the silane group and the cyan group are sequentially introduced into the nylon fiber,
(a) 실란화합물 5 내지 20 g/L, 및 산 0.1 내지 10 g/L를 포함하는 실란 수용액을 이용하여 나일론 섬유에 실란기를 도입하여 실란기 함유 나일론 섬유를 제조하는 단계; 및(a) preparing a silane group-containing nylon fiber by introducing a silane group into the nylon fiber using an silane solution containing 5 to 20 g / L of the silane compound and 0.1 to 10 g / L of acid; And
(b) 아크릴로니트릴 5 내지 50 g/L 및 산화환원 개시제 0.1 내지 10 g/L를 포함하는 수용액을 이용하여 실란기 함유 나일론 섬유 표면에 시안기가 도입된 나일론 섬유를 제조하는 단계; 및(b) preparing a nylon fiber having a cyan group introduced on the surface of the silane group-containing nylon fiber using an aqueous solution containing 5 to 50 g / L of acrylonitrile and 0.1 to 10 g / L of a redox initiator; And
(c) 구리 이온염 2.5 내지 50 g/L, 환원제 0.5 내지 20 g/L, 황화합물 1 내지 30 g/L, 및 pH 조절제 5 내지 45 g/L를 포함하는 황화구리 수용액을 이용하여 상기 실란기 및 시안기 함유 나일론 섬유에 황화구리를 흡착 또는 배위결합시키는 단계를 수행할 수 있다.(c) the silane group using a copper sulfide aqueous solution containing 2.5 to 50 g / L copper ion salt, 0.5 to 20 g / L reducing agent, 1 to 30 g / L sulfur compound, and 5 to 45 g / L pH adjuster. And adsorbing or coordinating copper sulfide to the cyan group-containing nylon fiber.
상기 (a)단계는 상기 실란 수용액 중에서 나일론 섬유를 30 내지 80 ℃로 0.1 내지 2시간 동안, 바람직하게 40 내지 60℃로 10분 내지 30분 동안 침지 후 여액의 실란 수용액을 제거하고 100 ℃로 유지시킨 건조기에 넣어 1 내지 2시간 건조하는 단계를 포함하는 것이 바람직하다.In the step (a), the nylon fibers are immersed in the silane solution at 30 to 80 ° C. for 0.1 to 2 hours, preferably at 40 to 60 ° C. for 10 minutes to 30 minutes, and then the silane solution of the filtrate is removed and maintained at 100 ° C. It is preferable to include a step of drying for 1 to 2 hours in the dryer.
또한, 상기 (b)의 시안기 도입 단계는 상기 아크릴로니트릴 수용액 중에서 실란기 함유 나일론 섬유를 50 내지 90 ℃로 1 내지 6시간, 바람직하게 60 내지 90 ℃로 2 내지 4시간 동안 반응을 진행시키는 것이 바람직하다.In addition, the cyan group introduction step of (b) is to proceed the reaction for 1 to 6 hours at 50 to 90 ℃, preferably 60 to 90 ℃ 2 to 4 hours the silane group-containing nylon fibers in the acrylonitrile aqueous solution It is preferable.
상기 (c)단계는 반응 효율 및 공정 시간 단축의 측면을 고려하여, 상기 황화구리 수용액 중에서 실란기 및 시안기 함유 나일론 섬유를 40 내지 90 ℃로 1 내지 24시간, 바람직하게 50 내지 70 ℃로 1 내지 6시간 동안 반응을 진행시키는 것이 바람직하다.In the step (c), the silane group and the cyan group-containing nylon fibers in the copper sulfide aqueous solution at 40 to 90 ° C. for 1 to 24 hours, preferably 50 to 70 ° C. in consideration of aspects of reaction efficiency and process time reduction. It is preferable to proceed with the reaction for from 6 hours.
또한, 상기 제2실시예의 도전성 나일론 섬유의 제조방법에 있어서, 나일론 섬유에 실란기 및 시안기를 동시에 도입하는 경우,In the method for producing the conductive nylon fiber of the second embodiment, when the silane group and the cyan group are simultaneously introduced into the nylon fiber,
실란화합물 5 내지 25 g/L, 산 0 내지 10 g/L, 아크릴로니트릴 5 내지 50 g/L 및 산화환원 개시제 0.1 내지 10 g/L를 포함하는 혼합 수용액을 이용하여 나일론 섬유 표면에 실란기 및 시안기를 동시에 도입하여 실란기 및 시안기 함유 나일론 섬유를 제조하는 단계; 및Silane group on the surface of nylon fiber using a mixed aqueous solution containing 5 to 25 g / L of silane compound, 0 to 10 g / L of acid, 5 to 50 g / L of acrylonitrile and 0.1 to 10 g / L of redox initiator And simultaneously introducing cyan groups to produce silane groups and cyan group-containing nylon fibers; And
구리 이온염 2.5 내지 50 g/L, 환원제 0.5 내지 20 g/L, 황화합물 1 내지 30 g/L, 및 pH 조절제 5 내지 45 g/L를 포함하는 황화구리 수용액을 이용하여 상기 실 란기 및 시안기 함유 나일론 섬유에 황화구리를 흡착 또는 배위결합시키는 단계를 수행할 수 있다.The silane group and cyan group using an aqueous copper sulfide solution containing 2.5 to 50 g / L of copper ion salt, 0.5 to 20 g / L of reducing agent, 1 to 30 g / L of sulfur compound, and 5 to 45 g / L of pH adjuster. The step of adsorbing or coordinating copper sulfide to the containing nylon fiber can be carried out.
본 발명에서 실란기 및 시안기 함유 나일론 섬유를 제조하는 단계는 상기 혼합 수용액 중에서 나일론 섬유를 60 내지 90 ℃로 1 내지 4시간 동안 반응을 진행시키는 것이 바람직하다.In the present invention, the preparing of the silane group and the cyan group-containing nylon fibers is preferably carried out the reaction for 1 to 4 hours at 60 to 90 ℃ nylon fibers in the mixed aqueous solution.
상기 실란기 및 시안기 함유 나일론 섬유에 황화구리를 흡착 또는 배위결합시키는 단계는 상기 황화구리 수용액 중에서 실란기 및 시안기 함유 나일론 섬유를 40 내지 90 ℃로 1 내지 24시간 동안 반응을 진행시키는 것이 바람직하다.The step of adsorbing or coordinating copper sulfide to the silane group and the cyan group-containing nylon fiber is preferably the reaction of the silane group and the cyan group-containing nylon fiber at 40 to 90 ° C. for 1 to 24 hours in the copper sulfide aqueous solution. Do.
상기 각 단계에서 사용되는 원료물질의 함량은 최적의 효과를 나타내기 위한 함량 범위를 한정한 것이므로, 상기 범위를 만족시키는 것이 실란기 및 시안기의 도입 및 황화구리의 흡착 및 배위결합 형성 측면에서 바람직하나, 본 발명이 반드시 상기 범위로만 한정되는 것은 아니다. Since the content of the raw material used in each step is limited to the content range for showing the optimum effect, it is preferable to satisfy the above range in terms of introduction of silane and cyanide and adsorption and coordination bond formation of copper sulfide. However, the present invention is not necessarily limited to the above range.
본 발명에서 사용되는 실란화합물은 아미노프로필트리에톡시실란, 아미노에틸아미노프로필트리메톡시실란, 비닐트리메톡시실란 및 비닐트리에톡시실란으로 이루어진 군에서 선택되는 1종 이상의 것이 바람직하다. 이때, 제1실시예의 경우 아미노프로필트리에톡시실란, 아미노에틸아미노프로필트리-메톡시실란 또는 이들의 혼합물을 사용하고, 제2실시예의 경우 비닐트리메톡시실란, 비닐트리에톡시실란 또는 이들의 혼합물을 사용하는 것이 보다 바람직하다.The silane compound used in the present invention is preferably one or more selected from the group consisting of aminopropyltriethoxysilane, aminoethylaminopropyltrimethoxysilane, vinyltrimethoxysilane and vinyltriethoxysilane. In this case, in the first embodiment, aminopropyltriethoxysilane, aminoethylaminopropyltri-methoxysilane, or a mixture thereof is used, and in the second embodiment, vinyltrimethoxysilane, vinyltriethoxysilane, or a combination thereof. It is more preferable to use mixtures.
또한, 상기 산은 황산, 염산, 아세트산 및 질산으로 이루어진 군에서 선택되 는 1종 이상인 것이 바람직하다.In addition, the acid is preferably at least one selected from the group consisting of sulfuric acid, hydrochloric acid, acetic acid and nitric acid.
상기 구리이온염은 2가 구리이온염을 사용하는 것이 바람직하고, 황산 제2구리, 염화 제2구리, 및 초산 제2구리로 이루어진 군에서 선택되는 1종 이상인 것이 더 바람직하다.It is preferable to use a divalent copper ion salt, and it is more preferable that the said copper ion salt is 1 or more types chosen from the group which consists of cupric sulfate, cupric chloride, and cupric acetate.
상기 산화환원 개시제는 라우로일 퍼옥사이드, 과산화수소, 과황산 칼륨, 과황산 암모늄, 아황산나트륨, 과황산 나트륨 및 과황산 알칼리 금속으로 이루어진 군에서 선택되는 1 종 이상인 것이 바람직하다.The redox initiator is preferably at least one selected from the group consisting of lauroyl peroxide, hydrogen peroxide, potassium persulfate, ammonium persulfate, sodium sulfite, sodium persulfate and alkali persulfate.
또한, 상기 환원제는 금속구리, 황산 제1철, 하이포인산나트륨, 산성아황산나트륨, 바나듐산 암모늄, 푸르푸랄 및 차아인산나트륨으로 이루어진 군에서 선택되는 1종 이상인 것이 바람직하다.In addition, the reducing agent is preferably at least one member selected from the group consisting of metal copper, ferrous sulfate, sodium hypophosphite, acidic sodium sulfite, ammonium vanadate, furfural and sodium hypophosphite.
상기 황화합물은 황화나트륨, 이산화황, 피로아황산나트륨, 티오황산나트륨, 황화수소 및 아황산으로 이루어진 군에서 선택되는 1종 이상인 것이 바람직하다.The sulfur compound is preferably at least one member selected from the group consisting of sodium sulfide, sulfur dioxide, sodium pyrosulfite, sodium thiosulfate, hydrogen sulfide and sulfite.
상기 pH 조절제는 황산, 염산, 초산, 및 구연산으로 이루어진 군에서 선택되는 1종 이상의 산과 탄산나트륨, 탄산칼슘, 가성소다, 인산나트륨, 아세트산나트륨 및 인산디나트륨으로 이루어진 군에서 선택되는 1종 이상의 염의 혼합물인 것이 바람직하다.The pH adjusting agent is a mixture of at least one acid selected from the group consisting of sulfuric acid, hydrochloric acid, acetic acid, and citric acid and at least one salt selected from the group consisting of sodium carbonate, calcium carbonate, sodium hydroxide, sodium phosphate, sodium acetate and disodium phosphate. Is preferably.
또한, 본 발명의 제1실시예 및 제2실시예에 따른 반응 공정 후에는 수세과정을 거치는 것이 바람직하며, 보다 바람직하게는 반응이 종료된 나일론 섬유를 상온의 물로 수차례 세척하고, 30 내지 80 ℃의 온수로 추가 세척한 후, 탈수 및 유제 처리하여 건조하는 방법으로 도전성 나일론 섬유를 제조할 수 있다. 다만, 상기 수세 공정은 최적의 공정을 예시한 것일 뿐, 본 발명이 상기 수세방법에 의해 한정되는 것은 아니며, 필요에 따라 다른 방법으로 수세할 수도 있음은 당연한 것이다.In addition, after the reaction process according to the first embodiment and the second embodiment of the present invention, it is preferable to go through a washing process, more preferably washed nylon several times with water at room temperature, the reaction is completed, 30 to 80 After further washing with warm water at ° C., a conductive nylon fiber can be produced by a method of drying by dehydration and emulsion treatment. However, the washing process is only an example of the optimal process, the present invention is not limited by the washing method, it is natural that washing may be performed by other methods as needed.
본 발명의 도전성 나일론 섬유는 간단한 화학반응을 통해 섬유표면에 실란기 또는 실란기와 시안기를 포함하고, 또한 상기 실란기와 시안기가 도전성이 우수한 황화구리의 흡착 또는 착물 형성을 용이하게 하여 우수한 도전성과 내세탁성을 가지게 하는 장점이 있다.The conductive nylon fiber of the present invention comprises a silane group or a silane group and a cyan group on the surface of the fiber through a simple chemical reaction, and the silane group and the cyan group facilitate the adsorption or complex formation of copper sulfide having excellent conductivity and excellent conductivity and washing resistance. It has the advantage of having sex.
이하, 본 발명의 바람직한 실시예를 기재한다. 다만, 하기의 실시예는 본 발명의 바람직한 일 실시예일 뿐, 본 발명이 하기 실시예에 의해 한정되는 것은 아니다.Hereinafter, preferred embodiments of the present invention are described. However, the following examples are only preferred embodiments of the present invention, and the present invention is not limited to the following examples.
비교예Comparative example 1 One
나일론 필라멘트사(70 데니어, 24 필라멘트, ㈜코오롱 제품)를 20g/L 황산제2구리, 5g/L 산성아황산나트륨 및 15g/L 티오황산나트륨이 포함되어 있고, 10g/L 구연산과 10g/L 인산디나트륨으로 pH가 3~4로 유지된 욕비 1:50의 혼합 수용액에 넣고 60℃로 가열하여 24시간 동안 처리하였다. 그런 다음, 처리된 필라멘트사를 상온의 물로 수차례 수세한 후, 다시 60℃ 물로 10분간 수세하고 탈수하여 90℃에 서 2시간 동안 건조시킴으로써, 5×101 Ωcm의 비저항을 갖는 담색의 올리브 블루 색의 섬유를 제조하였다.Nylon filament yarn (70 denier, 24 filament, manufactured by Kolon Corporation) contains 20 g / L cupric sulfate, 5 g / L sodium sulfite and 15 g / L sodium thiosulfate, and 10 g / L citric acid and 10 g / L phosphoric acid Sodium was added to a mixed aqueous solution of a bath ratio 1:50 maintained at a pH of 3 to 4 and heated to 60 ℃ was treated for 24 hours. Then, the treated filament yarn was washed several times with water at room temperature, and then washed with water at 60 ° C. for 10 minutes, dehydrated, and dried at 90 ° C. for 2 hours, whereby light blue olive blue having a resistivity of 5 × 10 1 Ωcm was obtained. Colored fibers were produced.
도전처리 전 섬유의 무게와 도전처리 후 섬유의 무게를 측정한 결과 제조되어진 나일론 도전성 섬유 내에 9.75 중량%의 황화구리가 흡착되었으며, 나일론 도전성 섬유를 회전드럼내의 비눗물에서 50℃로 유지하여 30분간 1회 세탁한 결과 9×103 Ωcm, 2회 세탁한 결과 106 Ωcm 이상으로 측정이 불가능할 정도의 비저항을 가지는 백색으로 완전히 탈색되었다.9.75% by weight of copper sulfide was adsorbed into the prepared nylon conductive fiber by measuring the weight of the fiber before the conductive treatment and the weight of the fiber after the conductive treatment. When washed twice, 9 × 10 3 Ωcm, two washes were completely discolored to white with a specific resistance of not more than 10 6 Ωcm.
실시예Example 1 One
나일론 필라멘트사(70 데니어, 24 필라멘트, ㈜코오롱 제품)를 10g/L 아미노프로필트리에톡시실란과 5g/L 황산이 포함되어 있는 욕비 1:50의 실란 수용액에 넣고, 40℃로 가열하여 30분간 침지하였다. 이후, 여액의 실란 수용액을 제거한 후, 필라멘트사를 100℃로 유지된 건조기에 넣고 1시간 동안 건조하여 섬유 표면에 실란기를 도입하였다.Nylon filament yarn (70 denier, 24 filament, Kolon Co., Ltd.) was put in an aqueous solution of 1:50 silane containing 10 g / L aminopropyltriethoxysilane and 5 g / L sulfuric acid and heated to 40 ° C. for 30 minutes. It was immersed. Then, after removing the silane aqueous solution of the filtrate, the filament yarn was put in a drier maintained at 100 ℃ and dried for 1 hour to introduce a silane group on the fiber surface.
실란기가 도입된 나일론 필라멘트사를 10g/L 황산제2구리, 1.5g/L 산성아황산나트륨 및 5g/L 티오황산나트륨이 포함되어 있고, 10g/L 구연산과 10g/L 인산디나트륨으로 pH가 3~4로 유지된 욕비 1:50의 혼합 수용액에 넣고 60℃로 가열하여 6시간 동안 처리하였다. 그런 다음, 처리된 필라멘트사를 상온의 물로 수차례 수세한 후, 다시 60℃ 물로 10분간 수세하고 탈수하여 90℃에서 2시간 동안 건조시킴으 로써, 2.5×101 Ωcm의 비저항을 갖는 담색의 올리브 블루 색의 섬유를 제조하였다.Nylon filament yarn with silane group contains 10 g / L cupric sulfate, 1.5 g / L sodium sulfite and 5 g / L sodium thiosulfate, and the pH is 3 ~ with 10 g / L citric acid and 10 g / L disodium phosphate. Into a mixed aqueous solution of the bath ratio 1:50 maintained at 4 and heated to 60 ℃ was treated for 6 hours. Then, the treated filament yarn was washed several times with water at room temperature, and then washed again with water at 60 ° C. for 10 minutes, dehydrated and dried at 90 ° C. for 2 hours, whereby light blue olive blue having a resistivity of 2.5 × 10 1 Ωcm was obtained. Colored fibers were produced.
SEM-EDS 분석 결과, 상기 전도성 섬유의 표면에는 1.5 중량%의 실란기가 도입되었으며, 도전처리 전 섬유의 무게와 도전처리 후 섬유의 무게를 측정한 결과 8.52 중량%의 황화구리를 포함하는 것을 확인하였다. 또한, 회전드럼내의 50℃ 비눗물에서 30분간 10회 세탁한 결과, 상기 전도성 섬유는 색상의 변화없이 1.9×102 Ωcm의 비저항을 나타내었다.As a result of SEM-EDS analysis, 1.5 wt% of the silane group was introduced to the surface of the conductive fiber, and the weight of the fiber before the conductive treatment and the weight of the fiber after the conductive treatment were found to include 8.52 wt% of copper sulfide. . In addition, as a result of washing for 10 minutes in 50 ℃ soapy water in a rotating drum, the conductive fiber showed a specific resistance of 1.9 × 10 2 Ωcm without changing the color.
실시예Example 2 2
상기의 실시예 1에 사용한 것과 동일한 나일론 필라멘트사를 30g/L 아미노프로필트리에톡시실란과 5g/L 황산이 포함되어 있는 욕비 1:50의 실란 수용액에 넣고 80℃로 가열하여 6시간 동안 반응시켜 탈수하였다. 이후, 실란기가 도입된 나일론 섬유를 10g/L 황산제2구리, 1.5g/L 산성아황산나트륨과 5g/L 티오황산나트륨이 포함되어 있고, 5g/L 아세트산과 10g/L 아세트산나트륨으로 pH가 4~5로 유지된 욕비 1:50의 혼합 수용액에 넣고, 60℃로 가열하여 6시간 동안 처리하였다. 그런 다음, 상온의 물로 수차례 수세한 후, 60℃ 물로 10분간 수세하고 탈수하여 90℃에서 2시간 동안 건조시킴으로써, 8×100 Ωcm의 비저항을 갖는 담색의 올리브 그린 색의 섬유를 제조하였다. 실시예 1과 동일한 방법으로 분석한 결과, 이 전도성 섬유는 0.98 중량%의 실란기가 도입되었으며, 10.2 중량%의 황화구리가 포함되어 있었다. 또한, 실시예 1과 동일한 조건에서 20회 세탁 후에도 색상의 변화는 없었으며 5.3 ×101 Ωcm의 비저항을 나타내었다.The same nylon filament yarn as used in Example 1 was added to an aqueous silane solution containing a ratio of 1:50 containing 30 g / L aminopropyltriethoxysilane and 5 g / L sulfuric acid, heated to 80 ° C., and reacted for 6 hours. Dehydrated. After that, the nylon fiber introduced with the silane group contains 10 g / L cupric sulfate, 1.5 g / L sodium sulfite and 5 g / L sodium thiosulfate, and the pH is 4 ~ 5 g / L acetic acid and 10 g / L sodium acetate. The mixture was put in a mixed aqueous solution having a bath ratio of 1:50 maintained at 5, and heated to 60 ° C. for 6 hours. Then, washed several times with water at room temperature, washed with water at 60 ℃ for 10 minutes, dehydrated and dried for 2 hours at 90 ℃, to prepare a light-colored olive green fiber having a specific resistance of 8 × 10 0 Ωcm. As a result of analysis in the same manner as in Example 1, this conductive fiber contained 0.98 wt% of silane groups and contained 10.2 wt% of copper sulfide. In addition, even after washing 20 times under the same conditions as in Example 1, there was no change in color and showed a resistivity of 5.3 × 10 1 Ωcm.
실시예Example 3 3
상기의 실시예 1에 사용한 것과 동일한 나일론 필라멘트사를 50g/L 아미노프로필트리에톡시실란과 5g/L 황산이 포함되어 있는 욕비 1:50의 실란 수용액에 넣고 40℃로 가열하여 24시간 동안 반응시켜 탈수하였다. 이후, 실란기가 도입된 나일론 섬유를 20g/L 황산제2구리, 10g/L 산성아황산나트륨과 10g/L 티오황산나트륨이 포함되어 있고, 10g/L 시트르산과 10g/L 디인산나트륨으로 pH가 3~4로 유지된 욕비 1:50의 혼합 수용액에 넣고 60℃로 가열하여 12시간 동안 처리하였다. 그런 다음, 상온의 물로 수차례 수세한 후, 60℃ 물로 10분간 수세하고 탈수하여 90℃에서 2시간 동안 건조시킴으로써, 1×100 Ωcm의 비저항을 갖는 올리브 블루 색의 섬유를 제조하였다. 실시예 1과 동일한 방법으로 분석한 결과, 이 전도성 섬유는 1.32 중량%의 실란기가 도입되었고, 11.2 중량%의 황화구리를 포함하였다. 또한, 실시예 1과 동일한 조건에서 20회 세탁 후 4.1×100 Ωcm의 비저항을 나타내었다.The same nylon filament yarn used in Example 1 was added to an aqueous silane solution of 1:50 silane containing 50 g / L aminopropyltriethoxysilane and 5 g / L sulfuric acid, heated to 40 ° C., and reacted for 24 hours. Dehydrated. Thereafter, the nylon fiber introduced with the silane group contains 20 g / L cupric sulfate, 10 g / L sodium sulfite and 10 g / L sodium thiosulfate, and the pH is 3 to 10 g / L citric acid and 10 g / L sodium phosphate. Into a mixed aqueous solution of the bath ratio 1:50 maintained at 4 and heated to 60 ℃ was treated for 12 hours. Then, to prepare a number of times washed with water after, olive blue color to washing with water 60 ℃ 10 min and dehydrated with a specific resistance of the drying for 2 hours at 90 ℃, 1 × 10 0 Ωcm fibers of room temperature water. As a result of analysis in the same manner as in Example 1, the conductive fiber had introduced 1.32% by weight of silane group and contained 11.2% by weight of copper sulfide. In addition, after washing 20 times under the same conditions as in Example 1, it showed a specific resistance of 4.1 × 10 0 Ωcm.
실시예Example 4 4
상기의 실시예 1에 사용한 것과 동일한 나일론 필라멘트사를 50g/L 아미노에틸아미프로필트리메톡시실란과 3g/L 염산이 포함되어 있는 욕비 1:50의 실란 수용액에 넣고 80℃로 가열하여 6시간 동안 반응시켜 실란기가 도입된 나일론 섬유를 제조하였다. 이후, 상기의 실시예 2와 같은 방법으로 처리하여 황화구리가 함입되도록 처리함으로써, 6×100 Ωcm의 비저항을 갖는 올리브 그린 색의 섬유를 제조하였다. 실시예 1과 동일한 방법으로 분석한 결과, 이 전도성 섬유는 0.8 중량%의 실란기가 도입되었으며, 7.5 중량%의 황화구리가 포함되어 있었다. 실시예 1과 동일한 조건에서 20회 세탁시험 결과 8.1×101 Ωcm의 비저항을 나타내었다.The same nylon filament yarn as used in Example 1 was added to an aqueous silane solution of 1:50 containing 50 g / L aminoethylamipropyl trimethoxysilane and 3 g / L hydrochloric acid, and heated to 80 ° C. for 6 hours. The reaction was performed to prepare nylon fibers into which a silane group was introduced. Thereafter, the same process as in Example 2 above was performed to include copper sulfide, thereby preparing olive green fibers having a specific resistance of 6 × 10 0 Ωcm. As a result of analysis in the same manner as in Example 1, 0.8 wt% of the silane group was introduced and 7.5 wt% of copper sulfide was included in the conductive fiber. 20 times of the laundry test under the same conditions as in Example 1 showed a specific resistance of 8.1 × 10 1 Ωcm.
실시예Example 5 5
상기의 실시예 1에 사용한 것과 동일한 나일론 필라멘트사를 10g/L 아미노프로필트리에톡시실란, 20g/L 아미노에틸아미프로필트리메톡시실란과 5g/L 황산이 포함되어 있는 욕비 1:50의 실란 수용액에 넣고 40℃로 가열하여 24시간 동안 반응시켜 실란기가 도입된 나일론 섬유를 제조하였다. 이후, 상기의 실시예 2와 같은 방법으로 처리하여 황화구리가 함입되도록 처리함으로써, 2.7×100 Ωcm의 비저항을 갖는 올리브 그린 색의 섬유를 제조하였다. 실시예 1과 동일한 방법으로 분석한 결과, 이 전도성 섬유는 2.1 중량%의 실란기가 도입되었으며, 12.7 중량%의 황화구리를 포함하였다.The same nylon filament yarn as used in Example 1 above was used in an aqueous silane solution at a ratio of 1:50 containing 10 g / L aminopropyltriethoxysilane, 20 g / L aminoethylamipropyltrimethoxysilane, and 5 g / L sulfuric acid. It was put in to and heated to 40 ℃ to react for 24 hours to prepare a nylon fiber introduced silane group. Thereafter, by treating the copper sulfide to be embedded in the same manner as in Example 2, to produce an olive green fiber having a specific resistance of 2.7 × 10 0 Ωcm. As a result of analysis in the same manner as in Example 1, this conductive fiber contained 2.1 wt% of silane group and contained 12.7 wt% of copper sulfide.
실시예Example 6 6
상기의 실시예 1에 사용한 것과 동일한 나일론 필라멘트사를 5g/L 비닐메톡시실란이 포함되어 있는 욕비 1:50의 실란 수용액에 넣고, 40℃로 가열하여 24시간 침지하였다. 이어서, 여액의 실란 수용액을 제거하고, 90℃로 유지된 건조기에 넣고 1시간 동안 건조하여 섬유 표면에 비닐기가 포함되어 있는 실란기를 도입하였다. 비닐 실란기가 도입된 나일론 필라멘트사를 50g/L 아크릴로니트릴, 5g/L 과황산 칼륨과 3g/L 아황산나트륨이 포함되어 있는 욕비 1:50의 혼합 수용액에 넣고 80℃로 가열하여 1시간 동안 처리하였다. 이후, 상온의 물로 수세하여 실란기 및 시안기가 도입된 나일론 섬유을 제조하였다. 실란기 및 시안기가 도입된 나일론 섬유를 10g/L 황산제2구리, 2g/L 산성아황산나트륨과 10g/L 티오황산나트륨이 포함되어 있고, 10g/L 아세트산과 25g/L 아세트산나트륨으로 pH가 4~5로 유지된 욕비 1:50의 혼합 수용액에 넣고 60℃로 가열하여 6시간 동안 처리하였다. 그리고, 상온의 물로 수차례 수세한 후, 60℃ 물로 10분간 수세하고 탈수하여 90℃에서 2시간 동안 건조시킴으로써, 2.5×101 Ωcm의 비저항을 갖는 담색의 올리브 그린 색의 섬유를 제조하였다. 실시예 1과 동일한 방법으로 분석한 결과, 이 전도성 섬유에는 1.8 중량%의 실란기가 도입되었음을 확인하였으며, FT-IR 분석을 통해 시안기의 특정피크(2240cm-1)가 새롭게 나타남을 확인하였다. 또한, 반응 전과 후의 섬유의 무게를 측정한 결과 1 중량%의 시안기를 포함하였으며, 황화구리 9.1 중량%가 포함되어 있었다. 제조된 나일론 도전성 섬유를 회전드럼내의 50℃ 비눗물에서 30분간 10회 세탁한 결과 색상의 변화없이 6.8×101 Ωcm의 비저항을 나타내었다.The same nylon filament yarn as used in Example 1 above was placed in an aqueous silane solution having a ratio of 1:50 containing 5 g / L vinylmethoxysilane, and heated to 40 ° C. for 24 hours. Subsequently, the silane aqueous solution of the filtrate was removed, placed in a dryer maintained at 90 ° C., and dried for 1 hour to introduce a silane group containing a vinyl group on the fiber surface. Nylon filament yarn with a vinyl silane group was introduced into a mixed aqueous solution of a bath ratio 1:50 containing 50 g / L acrylonitrile, 5 g / L potassium persulfate and 3 g / L sodium sulfite, and heated to 80 ° C. for 1 hour. It was. Thereafter, water was washed with water at room temperature to prepare a nylon fiber introduced with a silane group and a cyan group. 10g / L cupric sulfate, 2g / L sodium sulfite and 10g / L sodium thiosulfate are included in the nylon fiber in which the silane group and the cyan group are introduced, and the pH is 4 ~ with 10g / L acetic acid and 25g / L sodium acetate. It was added to a mixed aqueous solution of the bath ratio 1:50 maintained at 5 and heated to 60 ℃ was treated for 6 hours. After washing several times with water at room temperature, the resultant was washed with water at 60 ° C. for 10 minutes, dehydrated, and dried at 90 ° C. for 2 hours to prepare a pale olive green fiber having a specific resistance of 2.5 × 10 1 Ωcm. As a result of the analysis in the same manner as in Example 1, it was confirmed that 1.8 wt% of the silane group was introduced into the conductive fiber, and it was confirmed that the specific peak of the cyan group (2240 cm −1 ) appeared through FT-IR analysis. In addition, as a result of measuring the weight of the fiber before and after the reaction contained 1% by weight of the cyan group, it contained 9.1% by weight of copper sulfide. The prepared nylon conductive fiber was washed 10 times in 50 ° C soapy water in a rotating drum for 30 minutes It showed a specific resistance of 6.8 × 10 1 Ωcm without color change.
실시예Example 7 7
상기의 실시예 1에 사용한 것과 동일한 나일론 필라멘트사를 10g/L 비닐메톡시실란, 50g/L 아크릴로니트릴, 10g/L 과황산 칼륨과 5g/L 아황산나트륨 이 포함되어 있는 욕비 1:50의 혼합수용액에 넣고 60℃로 가열하여 2시간 동안 처리하였다. 이어서, 상온의 물로 수세하여 120℃로 유지된 건조기에 넣고 1시간 동안 건조하여 섬유 표면에 실란기 및 시안기를 동시에 도입하였다. 실란기 및 시안기가 도입된 나일론 필라멘트사를 상기의 실시예 6과 같은 방법으로 처리하여 황화구리가 함입되도록 처리함으로써, 3.8×101 Ωcm의 비저항을 갖는 담색의 올리브 그린 색의 섬유를 제조하였다. 실시예 1과 6과 동일한 방법으로 분석한 결과, 이 전도성 섬유는 0.62 중량%의 실란기가 도입되었으며, 1.8 중량%의 시안기 및 11.7 중량%의 황화구리가 포함되어 있었다. 실시예 6과 동일한 조건에서 20회 세탁시험 결과 1.2×102 Ωcm의 비저항을 나타내었다.The same nylon filament yarn used in Example 1 was mixed with a bath ratio of 1:50 containing 10 g / L vinylmethoxysilane, 50 g / L acrylonitrile, 10 g / L potassium persulfate and 5 g / L sodium sulfite The solution was added to an aqueous solution and heated to 60 ° C. for 2 hours. Subsequently, the resultant was washed with water at room temperature, placed in a drier maintained at 120 ° C., and dried for 1 hour to simultaneously introduce a silane group and a cyan group onto the fiber surface. The nylon filament yarn in which the silane group and the cyan group were introduced were treated in the same manner as in Example 6 to process copper sulfide to be incorporated, thereby preparing a light-colored olive green fiber having a specific resistance of 3.8 × 10 1 Ωcm. As a result of analysis in the same manner as in Examples 1 and 6, 0.62% by weight of the silane group was introduced, and the conductive fiber contained 1.8% by weight of the cyan group and 11.7% by weight of copper sulfide. 20 times of washing test under the same conditions as in Example 6 showed a specific resistance of 1.2 × 10 2 Ωcm.
실시예Example 8 8
상기의 실시예 1에 사용한 것과 동일한 나일론 필라멘트사를 10g/L 비닐에톡시실란과 2g/L 황산이 포함되어 있는 욕비 1:50의 실란 수용액에 넣고 40℃로 가열하여 24시간 침지하였다. 이어서, 여액의 실란 수용액을 제거하여 섬유 표면에 비닐기가 포함되어 있는 실란기를 도입하였다. 이것을 50g/L 아크릴로니트릴, 10g/L 과황산 칼륨과 10g/L 아황산나트륨이 포함되어 있는 욕비 1:50의 혼합 수용액에 넣고 80℃로 가열하여 2시간 동안 처리한 후 상온의 물로 수세하여 실란기 및 시안기 가 도입된 나일론 섬유을 제조하였다. 실란기 및 시안기가 도입된 나일론 섬유를 20g/L 황산제2구리, 5g/L 산성아황산나트륨과 15g/L 티오황산나트륨이 포함되어 있고, 10g/L 아세트산과 25g/L 아세트산나트륨으로 pH가 3~4로 유지된 욕비 1:50의 혼합 수용액에 넣고 60℃로 가열하여 12시간 동안 처리하였다. 그런 다음, 상온의 물로 수차례 수세한 후, 60℃ 물로 10분간 수세하고 탈수하여 90℃에서 2시간 동안 건조시킴으로써, 5×100 Ωcm의 비저항을 갖는 담색의 올리브 그린 색의 섬유를 제조하였다. 실시예 1과 6과 동일한 방법으로 분석한 결과, 이 전도성 섬유에는 1.4 중량%의 실란기가 도입되었으며, 0.8 중량%의 시안기 및 9.5 중량%의 황화구리를 포함하였다. 실시예 6과 동일한 조건에서 20회 세탁시험 결과 2.3×101 Ωcm의 비저항을 나타내었다.The same nylon filament yarn as used in Example 1 was put in an aqueous solution of silane at a ratio of 1:50 containing 10 g / L vinylethoxysilane and 2 g / L sulfuric acid, heated to 40 ° C., and soaked for 24 hours. Next, the silane aqueous solution of the filtrate was removed and the silane group in which the vinyl group was contained in the fiber surface was introduce | transduced. This was put into a mixed aqueous solution of 1:50 containing 50 g / L acrylonitrile, 10 g / L potassium persulfate and 10 g / L sodium sulfite, heated to 80 ° C. for 2 hours, washed with water at room temperature, and washed with silane. Nylon fibers in which groups and cyan groups were introduced were prepared. Nylon fiber incorporating silane and cyanide groups contains 20 g / L cupric sulfate, 5 g / L sodium sulfite and 15 g / L sodium thiosulfate, with 10 g / L acetic acid and 25 g / L sodium acetate. Into a mixed aqueous solution of the bath ratio 1:50 maintained at 4 and heated to 60 ℃ was treated for 12 hours. Then, washed several times with water at room temperature, washed with water at 60 ℃ for 10 minutes, dehydrated and dried for 2 hours at 90 ℃, to prepare a pale olive green fiber having a specific resistance of 5 × 10 0 Ωcm. As a result of analysis in the same manner as in Examples 1 and 6, 1.4 wt% of the silane group was introduced into the conductive fiber, and contained 0.8 wt% of the cyan group and 9.5 wt% of copper sulfide. 20 wash tests under the same conditions as in Example 6 showed a specific resistance of 2.3 × 10 1 Ωcm.
실시예Example 9 9
상기의 실시예 1에 사용한 것과 동일한 나일론 필라멘트사를 10g/L 비닐에톡시실란, 3g/L 황산, 50g/L 아크릴로니트릴, 10g/L 과황산 칼륨과 5g/L 아황산나트륨이 포함되어 있는 욕비 1:50의 혼합수용액에 넣고, 80℃로 가열하여 1시간 동안 처리하였다. 이어서, 상온의 물로 수세하여 120℃로 유지된 건조기에 넣고 1시간 동안 건조하여 섬유 표면에 실란기 및 시안기를 동시에 도입하였다. 실란기 및 시안기가 도입된 나일론 필라멘트사를 상기의 실시예 8과 같은 방법으로 처리하여 황화구리가 함입되도록 처리함으로써, 2.7×100 Ωcm의 비저항을 갖는 올리브 그린 색 의 섬유를 제조하였다. 실시예 1과 6과 동일한 방법으로 분석한 결과, 이 전도성 섬유는 0.89 중량%의 실란기가 도입되었으며, 1.1 중량%의 시안기 및 10.8 중량%의 황화구리가 포함되어 있었다.The same nylon filament yarn as that used in Example 1 was used as a bath ratio containing 10 g / L vinylethoxysilane, 3 g / L sulfuric acid, 50 g / L acrylonitrile, 10 g / L potassium persulfate and 5 g / L sodium sulfite It was put in a 1:50 mixed aqueous solution, and heated to 80 ° C. for 1 hour. Subsequently, the resultant was washed with water at room temperature, placed in a drier maintained at 120 ° C., and dried for 1 hour to simultaneously introduce a silane group and a cyan group onto the fiber surface. The nylon filament yarn in which the silane group and the cyan group were introduced were treated in the same manner as in Example 8 to process copper sulfide to be incorporated, thereby preparing an olive green fiber having a specific resistance of 2.7 × 10 0 Ωcm. As a result of analysis in the same manner as in Examples 1 and 6, 0.89 wt% of the silane group was introduced, and 1.1 wt% of the cyan group and 10.8 wt% of copper sulfide were included.
실시예Example 10 10
상기의 실시예 1에 사용한 것과 동일한 나일론 필라멘트사를 10 g/L 비닐메톡시실란, 10 g/L 비닐에톡시실란, 3 g/L 황산, 50 g/L 아크릴로니트릴, 10 g/L 과황산칼륨과 5 g/L 아황산나트륨이 포함되어 있는 욕비 1:50의 혼합수용액에 넣고 80℃로 가열하여 2시간 동안 처리하였다. 이어서, 상온의 물로 수세하여 120℃로 유지된 건조기에 넣고 1시간 동안 건조하여 섬유 표면에 실란기 및 시안기를 동시에 도입하였다. 실란기 및 시안기가 도입된 나일론 필라멘트사를 상기의 실시예 8과 같은 방법으로 처리하여 황화구리가 함입되도록 처리함으로써, 4×100 Ωcm의 비저항을 갖는 올리브 그린 색의 섬유를 제조하였다. 실시예 1과 6과 동일한 방법으로 분석한 결과, 이 전도성 섬유는 1.3 중량%의 실란기가 도입되었으며, 2 중량%의 시안기 및 13 중량%의 황화구리가 포함되어 있었다. 실시예 6과 동일한 조건에서 20회 세탁시험 결과 색상변화 없이 3.6×101 Ωcm의 비저항을 나타내었다.The same nylon filament yarn as used in Example 1 above was used with 10 g / L vinylmethoxysilane, 10 g / L vinylethoxysilane, 3 g / L sulfuric acid, 50 g / L acrylonitrile, 10 g / L The mixture was added to a mixed solution of a bath ratio 1:50 containing potassium sulfate and 5 g / L sodium sulfite, and heated to 80 ° C. for 2 hours. Subsequently, the resultant was washed with water at room temperature, placed in a drier maintained at 120 ° C., and dried for 1 hour to simultaneously introduce a silane group and a cyan group onto the fiber surface. The nylon filament yarn in which the silane group and the cyan group were introduced were treated in the same manner as in Example 8 to process copper sulfide to be incorporated to prepare an olive green fiber having a specific resistance of 4 × 10 0 Ωcm. As a result of analysis in the same manner as in Examples 1 and 6, 1.3 wt% of the silane group was introduced, and 2 wt% of the cyan group and 13 wt% of copper sulfide were included. 20 wash tests under the same conditions as in Example 6 showed a specific resistance of 3.6 × 10 1 Ωcm without color change.
이상에서 본 발명의 바람직한 실시예에 대하여 기재하였지만, 본 발명이 이에 한정되는 것은 아니고, 해당 기술 분야의 숙련된 기술자는 상기 기재된 범위 및 하기의 특허 청구범위에 기재된 본 발명의 사상 및 영역으로부터 벗어나지 않는 범위 내에서는 본 발명을 다양하게 변경 및 수정시킬 수 있음을 인지할 수 있을 것이다. Although the preferred embodiments of the present invention have been described above, the present invention is not limited thereto, and a person skilled in the art does not depart from the spirit and scope of the present invention described in the above-described range and the appended claims. It will be appreciated that various changes and modifications can be made within the scope of the invention.
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