WO2010029664A1 - 架橋アクリレート系繊維およびその製造方法 - Google Patents
架橋アクリレート系繊維およびその製造方法 Download PDFInfo
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- WO2010029664A1 WO2010029664A1 PCT/JP2009/002428 JP2009002428W WO2010029664A1 WO 2010029664 A1 WO2010029664 A1 WO 2010029664A1 JP 2009002428 W JP2009002428 W JP 2009002428W WO 2010029664 A1 WO2010029664 A1 WO 2010029664A1
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- Prior art keywords
- fiber
- crosslinked acrylate
- treatment
- fibers
- acrylonitrile
- Prior art date
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- 239000000835 fiber Substances 0.000 title claims abstract description 148
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 title claims abstract description 75
- 238000004519 manufacturing process Methods 0.000 title claims description 8
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 claims abstract description 63
- 238000011282 treatment Methods 0.000 claims abstract description 52
- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 claims abstract description 25
- NLHHRLWOUZZQLW-UHFFFAOYSA-N Acrylonitrile Chemical compound C=CC#N NLHHRLWOUZZQLW-UHFFFAOYSA-N 0.000 claims abstract description 23
- 150000002978 peroxides Chemical class 0.000 claims abstract description 20
- 230000007062 hydrolysis Effects 0.000 claims abstract description 10
- 238000006460 hydrolysis reaction Methods 0.000 claims abstract description 10
- JLVVSXFLKOJNIY-UHFFFAOYSA-N Magnesium ion Chemical compound [Mg+2] JLVVSXFLKOJNIY-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229910001425 magnesium ion Inorganic materials 0.000 claims abstract description 8
- 150000002500 ions Chemical class 0.000 claims abstract description 6
- 238000010521 absorption reaction Methods 0.000 claims description 32
- 238000000034 method Methods 0.000 claims description 14
- 150000002736 metal compounds Chemical class 0.000 claims description 13
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 11
- -1 hydrazine compound Chemical class 0.000 claims description 11
- 229910052749 magnesium Inorganic materials 0.000 claims description 11
- 239000011777 magnesium Substances 0.000 claims description 11
- 238000004132 cross linking Methods 0.000 claims description 8
- 229920006395 saturated elastomer Polymers 0.000 claims description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 4
- 239000001301 oxygen Substances 0.000 claims description 4
- 229910052760 oxygen Inorganic materials 0.000 claims description 4
- PTFCDOFLOPIGGS-UHFFFAOYSA-N Zinc dication Chemical compound [Zn+2] PTFCDOFLOPIGGS-UHFFFAOYSA-N 0.000 claims description 3
- 239000012770 industrial material Substances 0.000 abstract description 14
- 150000001875 compounds Chemical class 0.000 abstract description 2
- 150000001339 alkali metal compounds Chemical class 0.000 abstract 1
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 30
- 239000007864 aqueous solution Substances 0.000 description 25
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 20
- 159000000003 magnesium salts Chemical group 0.000 description 18
- 239000000243 solution Substances 0.000 description 15
- 238000011156 evaluation Methods 0.000 description 10
- YIXJRHPUWRPCBB-UHFFFAOYSA-N magnesium nitrate Chemical compound [Mg+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O YIXJRHPUWRPCBB-UHFFFAOYSA-N 0.000 description 10
- 159000000000 sodium salts Chemical class 0.000 description 10
- 230000000052 comparative effect Effects 0.000 description 8
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 6
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 6
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 description 6
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 6
- 229910052737 gold Inorganic materials 0.000 description 6
- 239000010931 gold Substances 0.000 description 6
- 229910052751 metal Inorganic materials 0.000 description 6
- 239000002184 metal Substances 0.000 description 6
- 229910017604 nitric acid Inorganic materials 0.000 description 6
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 5
- 150000003839 salts Chemical class 0.000 description 5
- 229910052708 sodium Inorganic materials 0.000 description 5
- 239000011734 sodium Substances 0.000 description 5
- 238000005406 washing Methods 0.000 description 5
- 238000007796 conventional method Methods 0.000 description 4
- 238000004043 dyeing Methods 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 239000000178 monomer Substances 0.000 description 4
- 125000002560 nitrile group Chemical group 0.000 description 4
- 229920000642 polymer Polymers 0.000 description 4
- 238000009987 spinning Methods 0.000 description 4
- 150000003751 zinc Chemical class 0.000 description 4
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 3
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 3
- 229910001870 ammonium persulfate Inorganic materials 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 239000003086 colorant Substances 0.000 description 3
- 238000003795 desorption Methods 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- 239000004745 nonwoven fabric Substances 0.000 description 3
- FUSNOPLQVRUIIM-UHFFFAOYSA-N 4-amino-2-(4,4-dimethyl-2-oxoimidazolidin-1-yl)-n-[3-(trifluoromethyl)phenyl]pyrimidine-5-carboxamide Chemical compound O=C1NC(C)(C)CN1C(N=C1N)=NC=C1C(=O)NC1=CC=CC(C(F)(F)F)=C1 FUSNOPLQVRUIIM-UHFFFAOYSA-N 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 2
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical group CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 description 2
- BAPJBEWLBFYGME-UHFFFAOYSA-N Methyl acrylate Chemical compound COC(=O)C=C BAPJBEWLBFYGME-UHFFFAOYSA-N 0.000 description 2
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 2
- DPOPAJRDYZGTIR-UHFFFAOYSA-N Tetrazine Chemical group C1=CN=NN=N1 DPOPAJRDYZGTIR-UHFFFAOYSA-N 0.000 description 2
- XTXRWKRVRITETP-UHFFFAOYSA-N Vinyl acetate Chemical compound CC(=O)OC=C XTXRWKRVRITETP-UHFFFAOYSA-N 0.000 description 2
- 125000003368 amide group Chemical group 0.000 description 2
- 230000000844 anti-bacterial effect Effects 0.000 description 2
- 229910052791 calcium Inorganic materials 0.000 description 2
- 239000011575 calcium Substances 0.000 description 2
- 229920001577 copolymer Polymers 0.000 description 2
- 238000002788 crimping Methods 0.000 description 2
- 239000002781 deodorant agent Substances 0.000 description 2
- 239000000706 filtrate Substances 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 229910000377 hydrazine sulfate Inorganic materials 0.000 description 2
- 239000012493 hydrazine sulfate Substances 0.000 description 2
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 2
- 229910052700 potassium Inorganic materials 0.000 description 2
- 239000011591 potassium Substances 0.000 description 2
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- VGTPCRGMBIAPIM-UHFFFAOYSA-M sodium thiocyanate Chemical compound [Na+].[S-]C#N VGTPCRGMBIAPIM-UHFFFAOYSA-M 0.000 description 2
- 239000011550 stock solution Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000000954 titration curve Methods 0.000 description 2
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 description 2
- ONDPHDOFVYQSGI-UHFFFAOYSA-N zinc nitrate Chemical compound [Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ONDPHDOFVYQSGI-UHFFFAOYSA-N 0.000 description 2
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 description 2
- 229960001763 zinc sulfate Drugs 0.000 description 2
- 229910000368 zinc sulfate Inorganic materials 0.000 description 2
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 description 1
- JAHNSTQSQJOJLO-UHFFFAOYSA-N 2-(3-fluorophenyl)-1h-imidazole Chemical group FC1=CC=CC(C=2NC=CN=2)=C1 JAHNSTQSQJOJLO-UHFFFAOYSA-N 0.000 description 1
- XEEYSDHEOQHCDA-UHFFFAOYSA-N 2-methylprop-2-ene-1-sulfonic acid Chemical compound CC(=C)CS(O)(=O)=O XEEYSDHEOQHCDA-UHFFFAOYSA-N 0.000 description 1
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 1
- MAGFQRLKWCCTQJ-UHFFFAOYSA-N 4-ethenylbenzenesulfonic acid Chemical compound OS(=O)(=O)C1=CC=C(C=C)C=C1 MAGFQRLKWCCTQJ-UHFFFAOYSA-N 0.000 description 1
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 description 1
- 229920002972 Acrylic fiber Polymers 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000010306 acid treatment Methods 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 229910000288 alkali metal carbonate Inorganic materials 0.000 description 1
- 150000008041 alkali metal carbonates Chemical class 0.000 description 1
- 150000008044 alkali metal hydroxides Chemical class 0.000 description 1
- 150000001340 alkali metals Chemical class 0.000 description 1
- 229910052784 alkaline earth metal Inorganic materials 0.000 description 1
- 150000001342 alkaline earth metals Chemical class 0.000 description 1
- BIVUUOPIAYRCAP-UHFFFAOYSA-N aminoazanium;chloride Chemical compound Cl.NN BIVUUOPIAYRCAP-UHFFFAOYSA-N 0.000 description 1
- 238000003321 atomic absorption spectrophotometry Methods 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- PTYMQUSHTAONGW-UHFFFAOYSA-N carbonic acid;hydrazine Chemical compound NN.OC(O)=O PTYMQUSHTAONGW-UHFFFAOYSA-N 0.000 description 1
- 125000002843 carboxylic acid group Chemical group 0.000 description 1
- 238000007334 copolymerization reaction Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 230000001877 deodorizing effect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 235000019253 formic acid Nutrition 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 230000020169 heat generation Effects 0.000 description 1
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 description 1
- 150000003840 hydrochlorides Chemical class 0.000 description 1
- 239000013067 intermediate product Substances 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- LVHBHZANLOWSRM-UHFFFAOYSA-N methylenebutanedioic acid Chemical group OC(=O)CC(=C)C(O)=O LVHBHZANLOWSRM-UHFFFAOYSA-N 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 150000002823 nitrates Chemical class 0.000 description 1
- 238000010979 pH adjustment Methods 0.000 description 1
- 229920002239 polyacrylonitrile Polymers 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 238000012805 post-processing Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- 229910001415 sodium ion Inorganic materials 0.000 description 1
- SQMCFUSVGSBKFK-UHFFFAOYSA-N sodium;5-(cyclohexen-1-yl)-1,5-dimethyl-1,3-diazinane-2,4,6-trione Chemical compound [Na+].O=C1N(C)C(=O)NC(=O)C1(C)C1=CCCCC1 SQMCFUSVGSBKFK-UHFFFAOYSA-N 0.000 description 1
- 125000000542 sulfonic acid group Chemical group 0.000 description 1
- 150000003467 sulfuric acid derivatives Chemical class 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- 239000011592 zinc chloride Substances 0.000 description 1
- 235000005074 zinc chloride Nutrition 0.000 description 1
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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
- D06M11/58—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 nitrogen or compounds thereof, e.g. with nitrides
- D06M11/63—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 nitrogen or compounds thereof, e.g. with nitrides with hydroxylamine or hydrazine
-
- 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
-
- 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
- D06M11/50—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 hydrogen peroxide or peroxides of metals; with persulfuric, permanganic, pernitric, percarbonic acids or their salts
-
- 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
- D06M2101/18—Synthetic fibres consisting of macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D06M2101/26—Polymers or copolymers of unsaturated carboxylic acids or derivatives thereof
- D06M2101/28—Acrylonitrile; Methacrylonitrile
-
- 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
-
- 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
- D06M2200/30—Flame or heat resistance, fire retardancy properties
Definitions
- the present invention relates to a crosslinked acrylate fiber and a method for producing the same. More specifically, the present invention relates to a crosslinked acrylate fiber having a color that does not cause discomfort in appearance even when used in combination with other fibers for industrial materials in the industrial material field.
- Cross-linked acrylate fibers are known to have various functions such as moisture absorption and desorption, moisture absorption exothermicity, deodorant properties, antibacterial properties, and flame retardancy, and are expected to expand into various fields. is there.
- moisture absorption and desorption moisture absorption exothermicity
- deodorant properties deodorant properties
- antibacterial properties antibacterial properties
- flame retardancy flame retardancy
- Patent Documents 1 to 3 have been studied to improve whiteness, and crosslinked acrylate fibers having practical whiteness are obtained.
- Patent Document 4 discloses black cross-linked acrylate-based fibers obtained using black original acrylic fibers as a raw material. Further, in Patent Documents 5 and 6, studies are made on various colors by dyeing crosslinked acrylate fibers. However, with respect to dyeing, further examination is necessary to make it practically sufficient in terms of hue stability, dyeing spots, dyeing fastness, and the like.
- the restrictions on the color of the crosslinked acrylate fiber cannot be ignored in the industrial material field.
- various types of industrial material fibers are often mixed and commercialized, and the color of such industrial material fibers is often similar to a gold color.
- the appearance of the product is uncomfortable.
- White is less uncomfortable than pink or black, but is costly and difficult to adopt because it takes many steps to improve whiteness.
- the conventional cross-linked acrylate fiber is in a situation where it is difficult to develop in the industrial material field, despite having various functions as described above.
- the cross-linked acrylate fiber has flame retardancy.
- the carboxyl group in the fiber is a magnesium salt type
- the cross-linked acrylate fiber is extremely high that is not found in general organic fiber. It is known to have flame retardancy (Patent Document 7).
- the magnesium salt type crosslinked acrylate fiber has a feature of slow moisture absorption / release, that is, a low moisture absorption / release rate (Patent Document 8). For this reason, continuous heat generation by moisture absorption is possible, which is particularly useful in the clothing field.
- magnesium salt-type crosslinked acrylate fibers cannot achieve both high flame retardancy and high moisture absorption / release rate, and cannot be developed for applications requiring such characteristics.
- An object of the present invention is a cross-linked acrylate which has an unfavorable appearance in color even in combination with other industrial material fibers in the industrial material field, which has not been provided in the prior art, and is advantageous in terms of cost. It is to provide a system fiber. Another object of the present invention is to provide a cross-linked acrylate fiber having both high flame retardancy and high moisture absorption / release rate.
- a crosslinking introduction treatment with a hydrazine compound for the acrylonitrile fiber, (a) a crosslinking introduction treatment with a hydrazine compound, (b) a peroxide treatment, (c) a hydrolysis treatment with an alkaline metal compound, (a), ( The crosslinked acrylate fiber according to [1], wherein the crosslinked acrylate fiber is obtained in the order of b), (c), or (a) and then (b) and (c).
- the crosslinked acrylate fiber is characterized in that at least some of the carboxyl groups have magnesium ions as counter ions, have a limiting oxygen index of 30 to 50, and a saturated moisture absorption of 20 to 60% by weight.
- the cross-linked acrylate fiber of the present invention has a color similar to a gold color, there is no sense of incongruity even when mixed with a fiber for industrial materials, and the number of manufacturing steps is small, so the cost can be suppressed. It can be suitably used in the field. Further, in the crosslinked acrylate fiber of the present invention, even when the magnesium salt type is adopted, it is possible to express a high moisture absorption / release rate, and the high flame retardance that could not be realized by the conventional crosslinked acrylate fiber. Since it is possible to achieve both high performance and a high moisture absorption / release rate, it becomes possible to develop applications where such characteristics are required.
- FIG. 1 shows the moisture absorption curves of the crosslinked acrylate fibers of Examples 1 and 2 and Comparative Examples 1 and 2.
- the present invention is described in detail below.
- the cross-linked acrylate fiber of the present invention has a color similar to a gold color not found in conventional cross-linked acrylate fibers, and does not cause a sense of incongruity even when mixed with fibers for industrial materials.
- such colors are represented by JIS-Z-8729 with L * of 60 to 75, a * of 5.0 to 14.5, and b * of 23.0 to 30.0.
- the color is preferably a color having L * of 65 to 75, a * of 7.0 to 13.0, and b * of 23.5 to 27.0.
- the crosslinked acrylate fiber of the present invention is obtained by subjecting the acrylonitrile fiber to (a) a crosslinking introduction treatment with a hydrazine compound, (b) a treatment with a peroxide, and (c) a hydrolysis treatment with an alkaline metal compound. Can be obtained in the order of (a), (b), (c), or (b) and (c) after applying (a).
- the acrylonitrile fiber employed in the present invention is produced from an acrylonitrile polymer according to a known method, and the composition of the polymer is preferably 40% by weight or more, more preferably Is 50% by weight or more, more preferably 80% by weight or more.
- a crosslinked structure is introduced into the fiber by reacting the nitrile group of the acrylonitrile copolymer that forms the acrylonitrile fiber with the hydrazine compound.
- the cross-linked structure greatly affects the fiber properties. If the copolymerization composition of acrylonitrile is too small, the cross-linked structure must be reduced, and the fiber properties may be insufficient. It becomes easy to obtain a favorable result by making a polymerization composition into the said range.
- copolymer components other than acrylonitrile in the acrylonitrile-based polymer include sulfonic acid group-containing monomers such as methallylsulfonic acid and p-styrenesulfonic acid, and salts thereof, and carboxylic acid groups such as (meth) acrylic acid and itaconic acid.
- examples thereof include monomers such as a monomer and a salt thereof, styrene, vinyl acetate, (meth) acrylic acid ester, (meth) acrylamide and the like, and are not particularly limited as long as the monomer is copolymerizable with acrylonitrile.
- the form of the acrylonitrile fiber employed in the present invention may be any form such as short fiber, tow, yarn, knitted fabric, non-woven fabric, etc., and may be employed as an intermediate product in the manufacturing process, waste fiber, or the like.
- the treatment (a) by treating the acrylonitrile fiber with a solution containing a hydrazine compound, the nitrile group of the acrylonitrile fiber reacts with hydrazine, and a crosslinked structure is formed in the fiber.
- the hydrazine-based compound include hydrazine hydrate, hydrazine hydrochloride, hydrazine sulfate, neutral hydrazine sulfate, and hydrazine carbonate.
- the treatment conditions include a method of immersing the acrylonitrile fiber in an aqueous solution to which the hydrazine compound is added so that the concentration of hydrazine is 3 to 40% by weight, and treating within 50 hours at 50 to 120 ° C. Can be mentioned.
- the fiber obtained by the treatment (a) is treated with a solution containing a peroxide.
- the color of the finally obtained crosslinked acrylate fiber can be made a color that approximates the gold color.
- the peroxide used for the treatment include hydrogen peroxide, ammonium persulfate, and potassium persulfate.
- the treatment conditions include soaking the fiber in an aqueous solution having a peroxide concentration of 1 to 15% by weight, preferably 3 to 8% by weight, and treating at 50 to 120 ° C. for 0.5 to 20 hours. . Prior to this treatment, it is desirable to thoroughly wash the fibers with water and remove as much of the chemical remaining in the treatment (a) as possible.
- Treatment (c) is a hydrolysis treatment with an alkaline metal compound.
- the nitrile group or amide group present in the fiber is hydrolyzed to form a carboxyl group.
- the carboxyl group is a factor that develops characteristics such as moisture absorption and desorption, moisture absorption exothermic property, and deodorant property in the crosslinked acrylate fiber.
- the total carboxyl group amount is 1 to 12 mmol / g, preferably 3 to 10 mmol / g, more preferably 3 to 8 mmol / g of carboxyl groups are formed.
- the amount of carboxyl groups formed can be adjusted depending on the processing conditions.
- an amide group is produced
- Examples of the alkaline metal compound used in the treatment (c) include alkali metal hydroxides such as sodium hydroxide and potassium hydroxide, and alkali metal carbonates such as sodium carbonate.
- Examples of the treatment conditions include immersing the fiber in an aqueous solution of an alkaline metal compound having a concentration of 1 to 10% by weight, preferably 1 to 5% by weight, and treating at 50 to 120 ° C. for 1 to 10 hours.
- the counter ion of the formed carboxyl group is a metal ion corresponding to the used alkaline metal compound.
- the crosslinked acrylate fiber of the present invention can be obtained. Further, nitrates, sulfates, hydrochlorides and the like can be obtained.
- Ion exchange treatment with metal salts acid treatment with nitric acid, sulfuric acid, hydrochloric acid, formic acid, etc., or pH adjustment treatment with alkaline metal compounds, etc., to give the carboxyl group in the fiber a desired salt-type carboxyl group or H-type carboxyl
- properties such as moisture absorption / release properties, moisture absorption exothermic properties, deodorizing properties, antibacterial properties, and flame retardancy by converting them into groups or mixing different types of salt-type carboxyl groups.
- the kind of metal constituting the base carboxyl group is one kind from alkali metals such as lithium, sodium and potassium, alkaline earth metals such as magnesium and calcium, and other metals such as manganese, copper, zinc and silver.
- alkali metals such as lithium, sodium and potassium
- alkaline earth metals such as magnesium and calcium
- other metals such as manganese, copper, zinc and silver.
- a plurality of types can be selected according to required characteristics.
- salt-type carboxyl groups such as sodium, potassium, magnesium and calcium are suitable.
- a conventional crosslinked acrylate fiber which is not subjected to peroxide treatment. Compared to the above, even if the metal type of the salt-type carboxyl group is the same and the saturated moisture absorption rate is the same, it has the feature that the moisture absorption rate can be increased relatively, and it exhibits better moisture absorption and desorption it can.
- a magnesium salt type carboxyl group or a zinc salt type carboxyl group as the salt type carboxyl group.
- the amount of these salt-type carboxyl groups is preferably 2 mmol / g or more as an absolute amount and 50% or more based on the total amount of carboxyl groups, and more preferably 2 mmol / g or more as an absolute amount and total amount.
- a crosslinked acrylate fiber having a magnesium salt-type carboxyl group can be obtained by immersing the fiber after the treatment (c) in an aqueous solution containing magnesium ions such as an aqueous magnesium nitrate solution. Moreover, when it is desired to control the amount of the magnesium salt type carboxyl group more accurately, the following method can also be employed.
- the fiber after the treatment (c) is immersed in an acid aqueous solution such as nitric acid so that all the carboxyl groups in the fiber are H-type carboxyl groups.
- the obtained fiber is immersed in an alkaline aqueous solution containing sodium ions such as an aqueous sodium hydroxide solution to convert the H-type carboxyl group into a sodium salt-type carboxyl group.
- the amount of carboxyl groups converted to the sodium salt type can be changed by adjusting the pH.
- a magnesium salt-type carboxyl group by immersing in an aqueous solution containing magnesium ions such as an aqueous magnesium nitrate solution.
- a sodium salt type carboxyl group is converted to a magnesium salt type carboxyl group, and an H type carboxyl group is hardly converted to a magnesium salt type carboxyl group. That is, it is possible to control the magnesium salt type carboxyl group amount by controlling the sodium salt type carboxyl group amount by adjusting the pH.
- the magnesium salt-type crosslinked acrylate fiber of the present invention obtained as described above has a flame retardancy equivalent to that of a conventionally known magnesium salt-type crosslinked acrylate fiber, and has a critical oxygen index of 30 to 50, Preferably 35-50 can be expressed. Further, the fiber has a saturated moisture absorption rate of 20 to 60% by weight, preferably 30 to 60% by weight, and the moisture absorption rate is the same for 5 minutes in a 20 ° C. and 65% RH atmosphere. Compared to the conventional magnesium salt-type crosslinked acrylate fiber having a high rate, it achieves both high flame retardancy and high moisture absorption rate, both of which have not been achieved before.
- the zinc salt type crosslinked acrylate fiber can be obtained in the same manner as the magnesium salt type crosslinked acrylate fiber described above.
- an aqueous solution containing zinc ions such as an aqueous zinc chloride solution, an aqueous zinc nitrate solution, or an aqueous zinc sulfate solution may be used in place of the aqueous solution containing magnesium ions such as the aqueous magnesium nitrate solution described above.
- the reason why a crosslinked acrylate fiber having a color similar to a gold color is obtained is not certain, but the pink color of the conventional crosslinked acrylate fiber is derived from a tetrazine ring structure formed by a crosslinking introduction treatment with a hydrazine compound. Therefore, it is presumed that the tetrazine ring structure was changed by the peroxide treatment in the present invention.
- Total amount of carboxyl groups About 1 g of a sufficiently dried sample is precisely weighed (W1 [g]), 200 ml of a 1 mol / l hydrochloric acid aqueous solution is added thereto, and the mixture is allowed to stand for 30 minutes, filtered through a glass filter, added with water and washed with water. After repeating this treatment three times, the filtrate is sufficiently washed with water until the pH of the filtrate becomes 5 or more. Next, after putting this sample in 200 ml of water and adding 1 mol / l hydrochloric acid aqueous solution to pH 2, a titration curve is obtained with a 0.1 mol / l sodium hydroxide aqueous solution according to a conventional method.
- the consumption amount (V1 [ml]) of an aqueous sodium hydroxide solution consumed by carboxyl groups is determined from the titration curve, and the total carboxyl group amount is calculated by the following formula.
- Total carboxyl group content [mmol / g] (0.1 ⁇ V1) / W1
- a sufficiently dried sample is precisely weighed and acid-decomposed with a mixed solution of concentrated sulfuric acid and concentrated nitric acid according to a conventional method, and then the metal contained in the form of a salt of a carboxyl group is quantified by atomic absorption spectrophotometry according to a conventional method.
- the amount of salt-type carboxyl groups is calculated by dividing by the atomic weight of the metal.
- LOI Litered oxygen index
- Example 1 A spinning stock solution was prepared by dissolving acrylonitrile-based polymer of 90% acrylonitrile and 10% methyl acrylate in 48% sodium thiocyanate aqueous solution, and spinning, washing, stretching, crimping and heat treatment were carried out according to ordinary methods. 9 dtex, 70 mm raw fiber was obtained. This raw fiber was immersed in a 15% hydrazine aqueous solution at a bath ratio of 1:10 and treated under conditions of 120 ° C. and 1 hour. The obtained fiber was washed with water, immersed in a 4% ammonium persulfate aqueous solution at a bath ratio of 1:10, and peroxide-treated at 100 ° C. for 1 hour.
- the obtained fiber is immersed in a 5% aqueous sodium hydroxide solution at a bath ratio of 1:10, hydrolyzed under conditions of 110 ° C. for 1 hour, and washed with water to obtain a sodium salt type crosslinked acrylate fiber. It was.
- the evaluation results of the properties of the obtained fiber are shown in Table 1 and FIG.
- Example 1 a sodium salt type crosslinked acrylate fiber was obtained in the same manner except that the peroxide treatment was not performed. The evaluation results of the properties of the obtained fiber are shown in Table 1 and FIG.
- Example 2 The crosslinked acrylate fiber obtained in Example 1 was treated with 1 mol / l nitric acid aqueous solution to convert the carboxyl group to H type, washed with water, adjusted to pH 12 with 1 mol / l sodium hydroxide, washed with water, sodium A fiber having a salt-type carboxyl group was obtained.
- an aqueous solution containing magnesium nitrate in an amount equivalent to 1.2 times the amount of carboxyl groups of the fiber, performing a conversion treatment to a magnesium salt type at 50 ° C. for 1 hour, and washing with water
- a magnesium salt type crosslinked acrylate fiber was obtained.
- the evaluation results of the properties of the obtained fiber are shown in Table 1 and FIG.
- Example 2 a magnesium salt type crosslinked acrylate fiber was obtained in the same manner except that the crosslinked acrylate fiber obtained in Comparative Example 1 was used in place of the crosslinked acrylate fiber obtained in Example 1. The evaluation results of the properties of the obtained fiber are shown in Table 1 and FIG.
- Example 3 sodium salt type crosslinked acrylate fiber was obtained in the same manner except that the peroxide treatment was performed with 3% hydrogen peroxide solution. Table 1 shows the evaluation results of the properties of the obtained fibers.
- Example 4 The raw material fiber employed in Example 1 was immersed in a 15% hydrazine aqueous solution at a bath ratio of 1:10, treated at 120 ° C. for 1 hour, and washed with water. The obtained fiber was immersed in an aqueous solution containing 4% ammonium persulfate and 5% sodium hydroxide at a bath ratio of 1:10, and simultaneous treatment with peroxide treatment and hydrolysis treatment at 100 ° C. for 1 hour. And washed with water to obtain a sodium salt type crosslinked acrylate fiber. The evaluation results of the properties of the obtained fiber are shown in Table 1.
- Example 5 A spinning stock solution in which acrylonitrile-based polymer of 88% acrylonitrile and 12% vinyl acetate was dissolved in 48% sodium thiocyanate aqueous solution was prepared, and spinning, washing, stretching, crimping and heat treatment were carried out in accordance with a conventional method, and 0.9 dtex was obtained. , 70 mm raw fiber was obtained. This raw fiber was immersed in a 15% aqueous hydrazine solution at a bath ratio of 1:10 and treated under conditions of 120 ° C. and 1.5 hours. The obtained fiber was washed with water, immersed in a 3% aqueous potassium persulfate solution at a bath ratio of 1:10, and peroxide-treated at 60 ° C.
- the obtained fiber is immersed in a 5% aqueous sodium hydroxide solution at a bath ratio of 1:10, hydrolyzed at 110 ° C. for 1 hour, and washed with water to obtain a sodium salt type crosslinked acrylate fiber. It was. Subsequently, the fiber is treated with a 1 mol / l nitric acid aqueous solution to convert the carboxyl group to H type, washed with water, adjusted to pH 12 with 1 mol / l sodium hydroxide, washed with water, and a fiber having a sodium salt type carboxyl group. Got.
- Example 6 The crosslinked acrylate fiber obtained in Example 1 was treated with 1 mol / l nitric acid aqueous solution to convert the carboxyl group to H type, washed with water, adjusted to pH 12 with 1 mol / l sodium hydroxide, washed with water, sodium A fiber having a salt-type carboxyl group was obtained. By immersing the fiber in an aqueous solution containing magnesium nitrate equivalent to 1.6 times the amount of carboxyl groups of the fiber, converting to a magnesium salt type at 50 ° C. for 1 hour, and washing with water A magnesium salt type crosslinked acrylate fiber was obtained. Table 1 shows the evaluation results of the properties of the obtained fibers.
- the crosslinked acrylate fibers of Comparative Examples 1 and 2 have a pink color, but the crosslinked acrylate fibers of Examples 1 to 6 subjected to peroxide treatment have a gold color. is there.
- the crosslinked acrylate fibers of Examples 1 and 2 have a lower amount of salt-type carboxyl groups than the crosslinked acrylate fibers of Comparative Examples 1 and 2, respectively, but 5 minutes from the start of moisture absorption. Looking at the moisture absorption rate later, in the case of the sodium salt type, it was 28% in Example 1 compared to 20% in Comparative Example 1, and in the case of the magnesium salt type, it was performed against 2% of Comparative Example 2. In Example 2, it is 6%, and the improvement in the moisture absorption rate is remarkable in the magnesium salt type.
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Abstract
Description
[1]JIS-Z-8729に記載の表示方法において、L*が60~75、a*が5.0~14.5、b*が23.0~30.0である色を有する架橋アクリレート系繊維。
[2]アクリロニトリル系繊維に対して、(a)ヒドラジン系化合物による架橋導入処理、(b)過酸化物による処理、(c)アルカリ性金属化合物による加水分解処理の各処理を、(a)、(b)、(c)の順に施すか、または、(a)を施した後、(b)および(c)を同時に施して得られることを特徴とする[1]に記載の架橋アクリレート系繊維。
[3]架橋アクリレート系繊維中の少なくとも一部のカルボキシル基がマグネシウムおよび/または亜鉛のイオンを対イオンとしていることを特徴とする[1]または[2]に記載の架橋アクリレート系繊維。
[4]架橋アクリレート系繊維中の少なくとも一部のカルボキシル基がマグネシウムイオンを対イオンとし、限界酸素指数が30~50であり、かつ飽和吸湿率が20~60重量%であることを特徴とする[3]に記載の架アクリレート系繊維。
[5]アクリロニトリル系繊維に対して、(a)ヒドラジン系化合物による架橋導入処理、(b)過酸化物による処理、(c)アルカリ性金属化合物による加水分解処理の各処理を、(a)、(b)、(c)の順に施すことを特徴とする架橋アクリレート系繊維の製造方法。
[6]アクリロニトリル系繊維に対して、(a)ヒドラジン系化合物による架橋導入処理、(b)過酸化物による処理、(c)アルカリ性金属化合物による加水分解処理の各処理を、(a)を施した後、(b)および(c)を同時に施すことを特徴とする架橋アクリレート系繊維の製造方法。
本発明の架橋アクリレート系繊維は、従来の架橋アクリレート系繊維にはないゴールド色に近似する色を有しており、産業資材用繊維と混用しても違和感を生じさせることがない。かかる色は、具体的には、JIS-Z-8729に記載の表示方法において、L*が60~75、a*が5.0~14.5、b*が23.0~30.0である色であり、L*が65~75、a*が7.0~13.0、b*が23.5~27.0である色であることが好ましい。
十分乾燥した試料約1gを精秤し(W1[g])、これに200mlの1mol/l塩酸水溶液を加え30分間放置したのちガラスフィルターで濾過し水を加えて水洗する。この処理を3回繰り返したのち、濾液のpHが5以上になるまで十分に水洗する。次にこの試料を200mlの水に入れ1mol/l塩酸水溶液を添加してpH2にした後、0.1mol/l水酸化ナトリウム水溶液で常法に従って滴定曲線を求める。該滴定曲線からカルボキシル基に消費された水酸化ナトリウム水溶液消費量(V1[ml])を求め、次式によって全カルボキシル基量を算出する。
全カルボキシル基量[mmol/g]=(0.1×V1)/W1
十分乾燥した試料を精秤し、常法に従って濃硫酸と濃硝酸の混合溶液で酸分解したのち、カルボキシル基の塩の形で含有される金属を常法に従って原子吸光光度法により定量し、該金属の原子量で除することにより塩型カルボキシル基量を算出する。
試料約5.0gを熱風乾燥器で105℃、16時間乾燥して重量を測定する(W2[g])。次に該試料を温度20℃、65%RHに調節した恒温恒湿器に24時間入れる。このようにして吸湿した試料の重量を測定する(W3[g])。以上の測定結果から、次式によって算出する。
飽和吸湿率[%]={(W3-W2)/W2}×100
試料約2.5gを熱風乾燥機で105℃、16時間乾燥して重量を測定する(W4[g])。続いて試料を円筒状メッシュカゴ(直径7.5cm、高さ9.8cm)に素早くふんわりとした状態となるように押し付けずに入れ、カゴごとすぐに20℃×65%RHに調節した恒温恒湿器に入れる。恒温恒湿器に入れた時点を吸湿開始時点として、5分、10分、20分および30分経過した時の吸湿した試料の重量を測定する(W5[g])。以上の測定結果から、次式によって各測定時点での吸湿率を算出し、吸湿曲線を求める。
吸湿率[%]={(W5-W4)/W4}×100
試料繊維を用いて目付180g/m2の不織布を作成し、該不織布に対してJIS-K-7201-2測定法に準拠してLOIを測定した。この数値が大きいほど難燃性が高いことを意味する。
解繊した試料をミノルタ株式会社製測色計CR300(D65光源)を用いて3回測色し、JIS-Z-8729に記載の表示方法によるL*、a*、b*のそれぞれの平均値を求める。
アクリロニトリル90%及びアクリル酸メチル10%のアクリロニトリル系重合体を48%のチオシアン酸ナトリウム水溶液で溶解した紡糸原液を作成し、常法に従って紡糸、水洗、延伸、捲縮、熱処理をして、0.9dtex、70mmの原料繊維を得た。この原料繊維を15%水加ヒドラジン水溶液に浴比1:10として浸漬し、120℃、1時間の条件で処理した。得られた繊維を水洗した後、4%過硫酸アンモニウム水溶液に浴比1:10として浸漬し、100℃、1時間の条件で過酸化物処理した。次いで、得られた繊維を、5%水酸化ナトリウム水溶液に浴比1:10として浸漬し、110℃、1時間の条件で加水分解し、水洗を行うことでナトリウム塩型架橋アクリレート系繊維を得た。得られた繊維の特性の評価結果を表1および図1に示す。
実施例1において、過酸化物処理を行わないこと以外は同様にして、ナトリウム塩型架橋アクリレート系繊維を得た。得られた繊維の特性の評価結果を表1および図1に示す。
実施例1で得られた架橋アクリレート系繊維を1mol/l硝酸水溶液で処理して、カルボキシル基をH型に変換し、水洗後、1mol/l水酸化ナトリウムでpH12に調整後、水洗し、ナトリウム塩型カルボキシル基を有する繊維を得た。該繊維を該繊維のカルボキシル基量の1.2倍等量の硝酸マグネシウムを含有する水溶液に浸漬し、50℃、1時間の条件でマグネシウム塩型への変換処理を行い、水洗を行うことでマグネシウム塩型架橋アクリレート系繊維を得た。得られた繊維の特性の評価結果を表1および図1に示す。
実施例2において、実施例1で得られた架橋アクリレート系繊維に代えて比較例1で得られた架橋アクリレート系繊維を用いること以外は同様にしてマグネシウム塩型架橋アクリレート系繊維を得た。得られた繊維の特性の評価結果を表1および図1に示す。
実施例1において、過酸化物処理を3%過酸化水素水で行うこと以外は同様にして、ナトリウム塩型架橋アクリレート系繊維を得た。得られた繊維の特性の評価結果を表1に示す。
実施例1で採用した原料繊維を15%水加ヒドラジン水溶液に浴比1:10として浸漬し、120℃、1時間の条件で処理し、水洗した。得られた繊維を4%の過硫酸アンモニウムと5%の水酸化ナトリウムを含有する水溶液に浴比1:10として浸漬し、100℃、1時間の条件で過酸化物処理・加水分解処理の同時処理を施し、水洗を行うことでナトリウム塩型架橋アクリレート系繊維を得た。得られた繊維の特性の評価結果を表1に示す。
アクリロニトリル88%及び酢酸ビニル12%のアクリロニトリル系重合体を48%のチオシアン酸ナトリウム水溶液で溶解した紡糸原液を作成し、常法に従って紡糸、水洗、延伸、捲縮、熱処理をして、0.9dtex、70mmの原料繊維を得た。この原料繊維を15%水加ヒドラジン水溶液に浴比1:10として浸漬し、120℃、1.5時間の条件で処理した。得られた繊維を水洗した後、3%過硫酸カリウム水溶液に浴比1:10として浸漬し、60℃、30分の条件で過酸化物処理した。次いで、得られた繊維を、5%水酸化ナトリウム水溶液に浴比1:10として浸漬し、110℃、1時間の条件で加水分解し、水洗を行うことでナトリウム塩型架橋アクリレート系繊維を得た。続いて該繊維を1mol/l硝酸水溶液で処理して、カルボキシル基をH型に変換し、水洗後、1mol/l水酸化ナトリウムでpH12に調整後、水洗し、ナトリウム塩型カルボキシル基を有する繊維を得た。該繊維を該繊維のカルボキシル基量の1.3倍等量の硫酸亜鉛を含有する水溶液に浸漬し、50℃、1時間の条件で亜鉛塩型への変換処理を行い、水洗を行うことで亜鉛塩型架橋アクリレート系繊維を得た。得られた繊維の特性の評価結果を表1に示す。
実施例1で得られた架橋アクリレート系繊維を1mol/l硝酸水溶液で処理して、カルボキシル基をH型に変換し、水洗後、1mol/l水酸化ナトリウムでpH12に調整後、水洗し、ナトリウム塩型カルボキシル基を有する繊維を得た。該繊維を該繊維のカルボキシル基量の1.6倍等量の硝酸マグネシウムを含有する水溶液に浸漬し、50℃、1時間の条件でマグネシウム塩型への変換処理を行い、水洗を行うことでマグネシウム塩型架橋アクリレート系繊維を得た。得られた繊維の特性の評価結果を表1に示す。
Claims (6)
- JIS-Z-8729に記載の表示方法において、L*が60~75、a*が5.0~14.5、b*が23.0~30.0である色を有する架橋アクリレート系繊維。
- アクリロニトリル系繊維に対して、(a)ヒドラジン系化合物による架橋導入処理、(b)過酸化物による処理、(c)アルカリ性金属化合物による加水分解処理の各処理を、(a)、(b)、(c)の順に施すか、または、(a)を施した後、(b)および(c)を同時に施して得られることを特徴とする請求項1に記載の架橋アクリレート系繊維。
- 架橋アクリレート系繊維中の少なくとも一部のカルボキシル基がマグネシウムおよび/または亜鉛のイオンを対イオンとしていることを特徴とする請求項1または2に記載の架橋アクリレート系繊維。
- 架橋アクリレート系繊維中の少なくとも一部のカルボキシル基がマグネシウムイオンを対イオンとし、限界酸素指数が30~50であり、かつ飽和吸湿率が20~60重量%であることを特徴とする請求項3に記載の架橋アクリレート系繊維。
- アクリロニトリル系繊維に対して、(a)ヒドラジン系化合物による架橋導入処理、(b)過酸化物による処理、(c)アルカリ性金属化合物による加水分解処理の各処理を、(a)、(b)、(c)の順に施すことを特徴とする架橋アクリレート系繊維の製造方法。
- アクリロニトリル系繊維に対して、(a)ヒドラジン系化合物による架橋導入処理、(b)過酸化物による処理、(c)アルカリ性金属化合物による加水分解処理の各処理を、(a)を施した後、(b)および(c)を同時に施すことを特徴とする架橋アクリレート系繊維の製造方法。
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TWI718890B (zh) * | 2010-10-06 | 2021-02-11 | 美商再生元醫藥公司 | 含有抗-介白素-4受體(il-4r)抗體之安定化配製物 |
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JP5056358B2 (ja) * | 2007-11-02 | 2012-10-24 | 日本エクスラン工業株式会社 | 可染性架橋アクリレート系繊維およびその製造方法ならびに該繊維を染色して得られる染色された架橋アクリレート系繊維 |
JP6228511B2 (ja) * | 2014-05-29 | 2017-11-08 | 日本エクスラン工業株式会社 | 分散性の良好な架橋アクリレート系繊維 |
KR102334183B1 (ko) * | 2016-09-26 | 2021-12-03 | 도요보 가부시키가이샤 | 흡습 발열성 섬유 |
TWI771378B (zh) * | 2017-03-23 | 2022-07-21 | 日商日本Exlan工業股份有限公司 | 吸溼性粒狀綿及含有該粒狀綿之中綿 |
JP7441429B2 (ja) | 2019-06-20 | 2024-03-01 | 日本エクスラン工業株式会社 | イオン交換繊維および該繊維を含有するイオン交換フィルター |
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JP4487083B2 (ja) | 2010-06-23 |
CN102066649B (zh) | 2013-05-15 |
KR20110053254A (ko) | 2011-05-19 |
EP2327831A1 (en) | 2011-06-01 |
JPWO2010029664A1 (ja) | 2012-02-02 |
CN102066649A (zh) | 2011-05-18 |
JP5029975B2 (ja) | 2012-09-19 |
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