JP5796922B1 - Polyester synthetic fiber treatment agent, polyester synthetic fiber treatment method, and polyester synthetic fiber - Google Patents
Polyester synthetic fiber treatment agent, polyester synthetic fiber treatment method, and polyester synthetic fiber Download PDFInfo
- Publication number
- JP5796922B1 JP5796922B1 JP2015104031A JP2015104031A JP5796922B1 JP 5796922 B1 JP5796922 B1 JP 5796922B1 JP 2015104031 A JP2015104031 A JP 2015104031A JP 2015104031 A JP2015104031 A JP 2015104031A JP 5796922 B1 JP5796922 B1 JP 5796922B1
- Authority
- JP
- Japan
- Prior art keywords
- polyester
- mass
- synthetic fiber
- phosphate
- metal salt
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- 229920000728 polyester Polymers 0.000 title claims abstract description 67
- 229920002994 synthetic fiber Polymers 0.000 title claims abstract description 58
- 239000012209 synthetic fiber Substances 0.000 title claims abstract description 58
- 239000003795 chemical substances by application Substances 0.000 title claims abstract description 45
- 238000000034 method Methods 0.000 title claims abstract description 35
- -1 alkali metal salt Chemical class 0.000 claims abstract description 71
- 229910019142 PO4 Inorganic materials 0.000 claims abstract description 30
- 229910052783 alkali metal Inorganic materials 0.000 claims abstract description 30
- 239000010452 phosphate Substances 0.000 claims abstract description 30
- 239000000835 fiber Substances 0.000 claims abstract description 28
- 239000002253 acid Substances 0.000 claims abstract description 17
- 125000000217 alkyl group Chemical group 0.000 claims abstract description 12
- 239000004094 surface-active agent Substances 0.000 claims abstract description 12
- 125000004432 carbon atom Chemical group C* 0.000 claims abstract description 10
- 238000012545 processing Methods 0.000 claims abstract description 9
- 229910001463 metal phosphate Inorganic materials 0.000 claims abstract description 8
- 150000003839 salts Chemical class 0.000 claims description 17
- RTZKZFJDLAIYFH-UHFFFAOYSA-N ether Substances CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 15
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 9
- NBIIXXVUZAFLBC-UHFFFAOYSA-L Phosphate ion(2-) Chemical compound OP([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-L 0.000 claims description 6
- 229910052751 metal Inorganic materials 0.000 claims description 6
- 239000002184 metal Substances 0.000 claims description 6
- 125000005702 oxyalkylene group Chemical group 0.000 claims description 5
- 125000006323 alkenyl amino group Chemical group 0.000 claims description 4
- 125000003282 alkyl amino group Chemical group 0.000 claims description 4
- 150000007522 mineralic acids Chemical class 0.000 claims description 4
- 229920000139 polyethylene terephthalate Polymers 0.000 claims description 4
- 239000005020 polyethylene terephthalate Substances 0.000 claims description 4
- 125000005037 alkyl phenyl group Chemical group 0.000 claims description 3
- 125000005907 alkyl ester group Chemical group 0.000 claims description 2
- 150000005215 alkyl ethers Chemical class 0.000 claims description 2
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims 1
- 230000015572 biosynthetic process Effects 0.000 claims 1
- 229910052698 phosphorus Inorganic materials 0.000 claims 1
- 239000011574 phosphorus Substances 0.000 claims 1
- 238000003672 processing method Methods 0.000 claims 1
- 238000003786 synthesis reaction Methods 0.000 claims 1
- 238000009825 accumulation Methods 0.000 abstract description 14
- 230000007423 decrease Effects 0.000 abstract description 5
- 230000007774 longterm Effects 0.000 abstract description 5
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 11
- 238000011156 evaluation Methods 0.000 description 11
- 239000007788 liquid Substances 0.000 description 10
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 6
- 239000000203 mixture Substances 0.000 description 6
- 239000000843 powder Substances 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 5
- 239000007864 aqueous solution Substances 0.000 description 5
- ZPWVASYFFYYZEW-UHFFFAOYSA-L dipotassium hydrogen phosphate Chemical compound [K+].[K+].OP([O-])([O-])=O ZPWVASYFFYYZEW-UHFFFAOYSA-L 0.000 description 5
- XAEFZNCEHLXOMS-UHFFFAOYSA-M potassium benzoate Chemical compound [K+].[O-]C(=O)C1=CC=CC=C1 XAEFZNCEHLXOMS-UHFFFAOYSA-M 0.000 description 5
- LWIHDJKSTIGBAC-UHFFFAOYSA-K tripotassium phosphate Chemical compound [K+].[K+].[K+].[O-]P([O-])([O-])=O LWIHDJKSTIGBAC-UHFFFAOYSA-K 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 4
- 238000007259 addition reaction Methods 0.000 description 4
- 125000003342 alkenyl group Chemical group 0.000 description 4
- BWIIMRFKCNBWEH-UHFFFAOYSA-L dipotassium;octadecyl phosphate Chemical compound [K+].[K+].CCCCCCCCCCCCCCCCCCOP([O-])([O-])=O BWIIMRFKCNBWEH-UHFFFAOYSA-L 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 4
- 238000009987 spinning Methods 0.000 description 4
- 125000001931 aliphatic group Chemical group 0.000 description 3
- 125000002947 alkylene group Chemical group 0.000 description 3
- 239000012298 atmosphere Substances 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 238000002788 crimping Methods 0.000 description 3
- 230000006866 deterioration Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 150000002148 esters Chemical class 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 125000006353 oxyethylene group Chemical group 0.000 description 3
- 229920006395 saturated elastomer Polymers 0.000 description 3
- 239000007921 spray Substances 0.000 description 3
- 239000012086 standard solution Substances 0.000 description 3
- 238000011144 upstream manufacturing Methods 0.000 description 3
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- POULHZVOKOAJMA-UHFFFAOYSA-N dodecanoic acid Chemical compound CCCCCCCCCCCC(O)=O POULHZVOKOAJMA-UHFFFAOYSA-N 0.000 description 2
- BXWNKGSJHAJOGX-UHFFFAOYSA-N hexadecan-1-ol Chemical compound CCCCCCCCCCCCCCCCO BXWNKGSJHAJOGX-UHFFFAOYSA-N 0.000 description 2
- IPCSVZSSVZVIGE-UHFFFAOYSA-N hexadecanoic acid Chemical compound CCCCCCCCCCCCCCCC(O)=O IPCSVZSSVZVIGE-UHFFFAOYSA-N 0.000 description 2
- 238000007654 immersion Methods 0.000 description 2
- SBOJXQVPLKSXOG-UHFFFAOYSA-N o-amino-hydroxylamine Chemical class NON SBOJXQVPLKSXOG-UHFFFAOYSA-N 0.000 description 2
- GLDOVTGHNKAZLK-UHFFFAOYSA-N octadecan-1-ol Chemical compound CCCCCCCCCCCCCCCCCCO GLDOVTGHNKAZLK-UHFFFAOYSA-N 0.000 description 2
- WWZKQHOCKIZLMA-UHFFFAOYSA-N octanoic acid Chemical compound CCCCCCCC(O)=O WWZKQHOCKIZLMA-UHFFFAOYSA-N 0.000 description 2
- WRKCIHRWQZQBOL-UHFFFAOYSA-N octyl dihydrogen phosphate Chemical compound CCCCCCCCOP(O)(O)=O WRKCIHRWQZQBOL-UHFFFAOYSA-N 0.000 description 2
- 230000000865 phosphorylative effect Effects 0.000 description 2
- CASUWPDYGGAUQV-UHFFFAOYSA-M potassium;methanol;hydroxide Chemical compound [OH-].[K+].OC CASUWPDYGGAUQV-UHFFFAOYSA-M 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- HLZKNKRTKFSKGZ-UHFFFAOYSA-N tetradecan-1-ol Chemical compound CCCCCCCCCCCCCCO HLZKNKRTKFSKGZ-UHFFFAOYSA-N 0.000 description 2
- DLYUQMMRRRQYAE-UHFFFAOYSA-N tetraphosphorus decaoxide Chemical compound O1P(O2)(=O)OP3(=O)OP1(=O)OP2(=O)O3 DLYUQMMRRRQYAE-UHFFFAOYSA-N 0.000 description 2
- 229910000404 tripotassium phosphate Inorganic materials 0.000 description 2
- 235000019798 tripotassium phosphate Nutrition 0.000 description 2
- ALSTYHKOOCGGFT-KTKRTIGZSA-N (9Z)-octadecen-1-ol Chemical compound CCCCCCCC\C=C/CCCCCCCCO ALSTYHKOOCGGFT-KTKRTIGZSA-N 0.000 description 1
- OYHQOLUKZRVURQ-NTGFUMLPSA-N (9Z,12Z)-9,10,12,13-tetratritiooctadeca-9,12-dienoic acid Chemical compound C(CCCCCCC\C(=C(/C\C(=C(/CCCCC)\[3H])\[3H])\[3H])\[3H])(=O)O OYHQOLUKZRVURQ-NTGFUMLPSA-N 0.000 description 1
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 description 1
- QGLWBTPVKHMVHM-KTKRTIGZSA-N (z)-octadec-9-en-1-amine Chemical compound CCCCCCCC\C=C/CCCCCCCCN QGLWBTPVKHMVHM-KTKRTIGZSA-N 0.000 description 1
- YIWUKEYIRIRTPP-UHFFFAOYSA-N 2-ethylhexan-1-ol Chemical compound CCCCC(CC)CO YIWUKEYIRIRTPP-UHFFFAOYSA-N 0.000 description 1
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 description 1
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 description 1
- DPUOLQHDNGRHBS-UHFFFAOYSA-N Brassidinsaeure Natural products CCCCCCCCC=CCCCCCCCCCCCC(O)=O DPUOLQHDNGRHBS-UHFFFAOYSA-N 0.000 description 1
- NTUUKSRCZOXNHM-UHFFFAOYSA-N CO.[O-2].[K+].[K+] Chemical compound CO.[O-2].[K+].[K+] NTUUKSRCZOXNHM-UHFFFAOYSA-N 0.000 description 1
- 239000005635 Caprylic acid (CAS 124-07-2) Substances 0.000 description 1
- 235000013162 Cocos nucifera Nutrition 0.000 description 1
- 244000060011 Cocos nucifera Species 0.000 description 1
- URXZXNYJPAJJOQ-UHFFFAOYSA-N Erucic acid Natural products CCCCCCC=CCCCCCCCCCCCC(O)=O URXZXNYJPAJJOQ-UHFFFAOYSA-N 0.000 description 1
- 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 1
- 239000005639 Lauric acid Substances 0.000 description 1
- IGFHQQFPSIBGKE-UHFFFAOYSA-N Nonylphenol Natural products CCCCCCCCCC1=CC=C(O)C=C1 IGFHQQFPSIBGKE-UHFFFAOYSA-N 0.000 description 1
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 1
- REYJJPSVUYRZGE-UHFFFAOYSA-N Octadecylamine Chemical compound CCCCCCCCCCCCCCCCCCN REYJJPSVUYRZGE-UHFFFAOYSA-N 0.000 description 1
- 239000005642 Oleic acid Substances 0.000 description 1
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 description 1
- 235000021314 Palmitic acid Nutrition 0.000 description 1
- 239000002202 Polyethylene glycol Substances 0.000 description 1
- GOOHAUXETOMSMM-UHFFFAOYSA-N Propylene oxide Chemical group CC1CO1 GOOHAUXETOMSMM-UHFFFAOYSA-N 0.000 description 1
- 229910004856 P—O—P Chemical group 0.000 description 1
- 235000021355 Stearic acid Nutrition 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 150000008044 alkali metal hydroxides Chemical class 0.000 description 1
- 150000003973 alkyl amines Chemical class 0.000 description 1
- 150000001495 arsenic compounds Chemical class 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 229960000541 cetyl alcohol Drugs 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 230000001143 conditioned effect Effects 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 150000005690 diesters Chemical group 0.000 description 1
- ZBCBWPMODOFKDW-UHFFFAOYSA-N diethanolamine Chemical class OCCNCCO ZBCBWPMODOFKDW-UHFFFAOYSA-N 0.000 description 1
- GWTCIAGIKURVBJ-UHFFFAOYSA-L dipotassium;dodecyl phosphate Chemical compound [K+].[K+].CCCCCCCCCCCCOP([O-])([O-])=O GWTCIAGIKURVBJ-UHFFFAOYSA-L 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- LQZZUXJYWNFBMV-UHFFFAOYSA-N dodecan-1-ol Chemical compound CCCCCCCCCCCCO LQZZUXJYWNFBMV-UHFFFAOYSA-N 0.000 description 1
- JRBPAEWTRLWTQC-UHFFFAOYSA-N dodecylamine Chemical compound CCCCCCCCCCCCN JRBPAEWTRLWTQC-UHFFFAOYSA-N 0.000 description 1
- 229920001971 elastomer Polymers 0.000 description 1
- 238000004945 emulsification Methods 0.000 description 1
- 239000003995 emulsifying agent Substances 0.000 description 1
- DPUOLQHDNGRHBS-KTKRTIGZSA-N erucic acid Chemical compound CCCCCCCC\C=C/CCCCCCCCCCCC(O)=O DPUOLQHDNGRHBS-KTKRTIGZSA-N 0.000 description 1
- 150000002170 ethers Chemical class 0.000 description 1
- 229940093920 gynecological arsenic compound Drugs 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 description 1
- 239000012046 mixed solvent Substances 0.000 description 1
- 229940043348 myristyl alcohol Drugs 0.000 description 1
- WQEPLUUGTLDZJY-UHFFFAOYSA-N n-Pentadecanoic acid Natural products CCCCCCCCCCCCCCC(O)=O WQEPLUUGTLDZJY-UHFFFAOYSA-N 0.000 description 1
- GOQYKNQRPGWPLP-UHFFFAOYSA-N n-heptadecyl alcohol Natural products CCCCCCCCCCCCCCCCCO GOQYKNQRPGWPLP-UHFFFAOYSA-N 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- SNQQPOLDUKLAAF-UHFFFAOYSA-N nonylphenol Chemical compound CCCCCCCCCC1=CC=CC=C1O SNQQPOLDUKLAAF-UHFFFAOYSA-N 0.000 description 1
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 1
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 description 1
- UHGIMQLJWRAPLT-UHFFFAOYSA-N octadecyl dihydrogen phosphate Chemical compound CCCCCCCCCCCCCCCCCCOP(O)(O)=O UHGIMQLJWRAPLT-UHFFFAOYSA-N 0.000 description 1
- IOQPZZOEVPZRBK-UHFFFAOYSA-N octan-1-amine Chemical compound CCCCCCCCN IOQPZZOEVPZRBK-UHFFFAOYSA-N 0.000 description 1
- 229960002446 octanoic acid Drugs 0.000 description 1
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 description 1
- 235000021313 oleic acid Nutrition 0.000 description 1
- 229940055577 oleyl alcohol Drugs 0.000 description 1
- XMLQWXUVTXCDDL-UHFFFAOYSA-N oleyl alcohol Natural products CCCCCCC=CCCCCCCCCCCO XMLQWXUVTXCDDL-UHFFFAOYSA-N 0.000 description 1
- 239000012188 paraffin wax Substances 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 229920001451 polypropylene glycol Polymers 0.000 description 1
- 229920002215 polytrimethylene terephthalate Polymers 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- WBHHMMIMDMUBKC-XLNAKTSKSA-N ricinelaidic acid Chemical compound CCCCCC[C@@H](O)C\C=C\CCCCCCCC(O)=O WBHHMMIMDMUBKC-XLNAKTSKSA-N 0.000 description 1
- 229960003656 ricinoleic acid Drugs 0.000 description 1
- FEUQNCSVHBHROZ-UHFFFAOYSA-N ricinoleic acid Natural products CCCCCCC(O[Si](C)(C)C)CC=CCCCCCCCC(=O)OC FEUQNCSVHBHROZ-UHFFFAOYSA-N 0.000 description 1
- 238000007378 ring spinning Methods 0.000 description 1
- 150000004671 saturated fatty acids Chemical class 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 241000894007 species Species 0.000 description 1
- 239000008117 stearic acid Substances 0.000 description 1
- 229940012831 stearyl alcohol Drugs 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- TUNFSRHWOTWDNC-HKGQFRNVSA-N tetradecanoic acid Chemical compound CCCCCCCCCCCCC[14C](O)=O TUNFSRHWOTWDNC-HKGQFRNVSA-N 0.000 description 1
- KRIXEEBVZRZHOS-UHFFFAOYSA-N tetradecyl dihydrogen phosphate Chemical compound CCCCCCCCCCCCCCOP(O)(O)=O KRIXEEBVZRZHOS-UHFFFAOYSA-N 0.000 description 1
- 238000004448 titration Methods 0.000 description 1
- 235000021122 unsaturated fatty acids Nutrition 0.000 description 1
- 150000004670 unsaturated fatty acids Chemical class 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
- 239000008096 xylene Substances 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
- 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
- D06M13/282—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 with compounds containing phosphorus
- D06M13/292—Mono-, di- or triesters of phosphoric or phosphorous acids; Salts 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
- D06M11/68—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 phosphorus or compounds thereof, e.g. with chlorophosphonic acid or salts thereof
- D06M11/70—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 phosphorus or compounds thereof, e.g. with chlorophosphonic acid or salts thereof with oxides of phosphorus; with hypophosphorous, phosphorous or phosphoric acids or their salts
- D06M11/71—Salts of phosphoric acids
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/10—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing oxygen
- D06M13/165—Ethers
- D06M13/17—Polyoxyalkyleneglycol ethers
-
- 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
- D06M13/368—Hydroxyalkylamines; Derivatives thereof, e.g. Kritchevsky bases
-
- 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
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/53—Polyethers
-
- 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
- D06M2101/32—Polyesters
Landscapes
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
- Chemical Or Physical Treatment Of Fibers (AREA)
Abstract
【課題】ポリエステル系合成繊維の製造工程における延伸性不良、練条工程でのスカム堆積、加工工程での糸品位低下、更には長期在庫に伴う繊維強度の低下等を抑制できるポリエステル系合成繊維用処理剤、かかる処理剤を用いるポリエステル系合成繊維の処理方法及びかかる処理方法により得られるポリエステル系合成繊維を提供する。【解決手段】ポリエステル系合成繊維用処理剤として、分子中に炭素数12〜22のアルキル基を有するアルキルリン酸エステルのアルカリ金属塩を40〜80質量%、特定の界面活性剤を20〜59.99質量%及び特定のリン酸金属塩を0.01〜3.0質量%(合計100質量%)の割合で含有して成り、アルキルリン酸エステルのアルカリ金属塩の酸価が0.1〜90KOHmg/gであるものを用いた。【選択図】なしAn object of the present invention is to provide polyester-based synthetic fibers that can suppress poor stretchability in the production process of polyester-based synthetic fibers, scum accumulation in the drawing process, lower yarn quality in the processing process, and further decrease in fiber strength due to long-term inventory. A treating agent, a method for treating a polyester synthetic fiber using such a treating agent, and a polyester synthetic fiber obtained by such a treating method are provided. As a treatment agent for polyester-based synthetic fibers, 40-80% by mass of an alkali metal salt of an alkyl phosphate having an alkyl group having 12 to 22 carbon atoms in the molecule, and a specific surfactant is 20-59. .99% by mass and a specific metal phosphate in a proportion of 0.01 to 3.0% by mass (total 100% by mass), and the acid value of the alkali metal salt of the alkyl phosphate is 0.1. What was -90KOHmg / g was used. [Selection figure] None
Description
本発明は、ポリエステル系合成繊維用処理剤、かかる処理剤を用いるポリエステル系合成繊維の処理方法及びかかる処理方法により得られるポリエステル系合成繊維に関する。 The present invention relates to a polyester synthetic fiber treatment agent, a polyester synthetic fiber treatment method using such a treatment agent, and a polyester synthetic fiber obtained by the treatment method.
従来、ポリエステル系合成繊維用処理剤として、アルキルリン酸エステルのカリウム塩及びアルキルアミン類を特定割合で含有して成るもの(例えば、特許文献1参照)、有機リン酸エステル塩及びオキシアルキレンポリマーを特定割合で含有して成るもの(例えば、特許文献2参照)、アルキルリン酸エステルのカリウム塩、パラフィンワックス及び乳化剤を特定割合で含有して成るもの(例えば、特許文献3参照)等が提案されている。しかし、これら従来のポリエステル系合成繊維用処理剤には、ポリエステル系合成繊維の製造工程における延伸時に延伸性不良による糸切れがしばしば起こるという問題があり、また近年の紡績工程の高速化に対応できず、練条工程にてスカムが堆積したり、加工工程で白粉発生を伴う糸切れや糸品位低下が起こり、更に長期在庫に伴う繊維強度の低下が起こるという問題もある。 Conventionally, as a treatment agent for polyester-based synthetic fibers, an alkyl phosphate ester potassium salt and an alkylamine containing a specific ratio (for example, see Patent Document 1), an organic phosphate ester salt, and an oxyalkylene polymer Proposed in a specific ratio (for example, refer to Patent Document 2), and those that include a potassium salt of an alkyl phosphate ester, paraffin wax and an emulsifier in a specific ratio (for example, refer to Patent Document 3). ing. However, these conventional polyester synthetic fiber treatment agents have a problem that yarn breakage often occurs due to poor stretchability during stretching in the production process of polyester synthetic fibers, and can cope with the recent increase in spinning process speed. In addition, there is a problem that scum accumulates in the drawing process, yarn breakage or deterioration of the yarn quality accompanied by generation of white powder occurs in the processing process, and fiber strength decreases due to long-term inventory.
本発明が解決しようとする課題は、ポリエステル系合成繊維の製造工程における延伸性不良、練条工程でのスカム堆積、加工工程での糸品位低下、更には長期在庫に伴う繊維強度の低下等を抑制できるポリエステル系合成繊維用処理剤、かかる処理剤を用いるポリエステル系合成繊維の処理方法及びかかる処理方法により得られるポリエステル系合成繊維を提供する処にある。 The problems to be solved by the present invention include poor stretchability in the production process of polyester-based synthetic fibers, scum accumulation in the drawing process, lower yarn quality in the processing process, and lower fiber strength due to long-term inventory. The present invention is to provide a polyester synthetic fiber treatment agent that can be suppressed, a polyester synthetic fiber treatment method using such a treatment agent, and a polyester synthetic fiber obtained by such a treatment method.
本発明者らは、前記の課題を解決するべく研究した結果、特定の3成分を特定割合で含有して成るポリエステル系合成繊維用処理剤が正しく好適であることを見出した。 As a result of researches to solve the above-mentioned problems, the present inventors have found that a polyester synthetic fiber treatment agent containing specific three components in a specific ratio is correctly suitable.
すなわち本発明は、分子中に炭素数12〜22のアルキル基を有するアルキルリン酸エステルのアルカリ金属塩を40〜80質量%、下記の界面活性剤を20〜59.99質量%及び下記のリン酸金属塩を0.01〜3.0質量%(合計100質量%)の割合で含有して成り、アルキルリン酸エステルのアルカリ金属塩の酸価が0.1〜90KOHmg/gであるポリエステル系合成繊維用処理剤に係る。また本発明は、かかるポリエステル系合成繊維用処理剤を用いるポリエステル系合成繊維の処理方法、かかる処理方法により得られるポリエステル系合成繊維に係る。 That is, the present invention relates to an alkali metal salt of an alkyl phosphate having an alkyl group having 12 to 22 carbon atoms in the molecule, 40 to 80% by mass of the following surfactant, and 20 to 59.99% by mass of the following surfactant. A polyester system comprising an acid metal salt in a proportion of 0.01 to 3.0% by mass (total of 100% by mass), wherein the acid value of the alkali metal salt of the alkyl phosphate ester is 0.1 to 90 KOHmg / g It relates to a treating agent for synthetic fibers. The present invention also relates to a polyester synthetic fiber treatment method using such a polyester synthetic fiber treating agent, and a polyester synthetic fiber obtained by such a treatment method.
界面活性剤:ポリオキシアルキレンアルキルエーテル、ポリオキシアルキレンアルケニルエーテル、ポリオキシアルキレンアルキルエステル、ポリオキシアルキレンアルケニルエステル、ポリオキシアルキレンアルキルフェニルエーテル、ポリオキシアルキレンアルキルアミノエーテル、ポリオキシアルキレンアルケニルアミノエーテル、ポリオキシアルキレンアルキルアミノエーテルと無機酸との塩及びポリオキシアルキレンアルケニルアミノエーテルと無機酸との塩から選ばれる少なくとも一つ Surfactant: polyoxyalkylene alkyl ether, polyoxyalkylene alkenyl ether, polyoxyalkylene alkyl ester, polyoxyalkylene alkenyl ester, polyoxyalkylene alkyl phenyl ether, polyoxyalkylene alkyl amino ether, polyoxyalkylene alkenyl amino ether, poly At least one selected from a salt of an oxyalkylene alkylamino ether and an inorganic acid and a salt of a polyoxyalkylene alkenyl amino ether and an inorganic acid
リン酸金属塩:リン酸水素二金属塩及びリン酸三金属塩から選ばれる少なくとも一つ Metal phosphate: at least one selected from bimetallic hydrogen phosphate and trimetallic phosphate
先ず、本発明に係るポリエステル系合成繊維用処理剤(以下、本発明の処理剤という)について説明する。本発明の処理剤に供する分子中に炭素数12〜22のアルキル基を有するアルキルリン酸エステルのアルカリ金属塩としては、ドデシルリン酸エステルアルカリ金属塩、トリデシルリン酸エステルアルカリ金属塩、ミリスチルリン酸エステルアルカリ金属塩、ヘキサデシルリン酸エステルアルカリ金属塩、オクタデシルリン酸エステルアルカリ金属塩、イソステアリルリン酸エステルアルカリ金属塩、ドコシルリン酸エステルアルカリ金属塩等が挙げられるが、なかでもヘキサデシルリン酸エステルアルカリ金属塩、オクタデシルリン酸エステルアルカリ金属塩等の、アルキルリン酸エステルのアルカリ金属塩中のアルキル基が炭素数16〜18のものが好ましい。これらのアルキルリン酸エステルアルカリ金属塩は脂肪族1価アルコールと無水リン酸に代表されるリン酸化剤との反応、及びその後のアルカリ金属水酸化物との中和反応により合成されるが、用いる脂肪族1価アルコールは単一成分でも2種以上の成分の混合物でもよい。また一般にアルキルリン酸エステルのアルカリ金属塩は、モノエステル、ジエステル及びP−O−P結合を含むポリ体からなる混合物であるが、その構成比率は特に制限されない。またアルカリ金属塩としてはカリウム塩が好ましい。合成原料に含まれる不純物については、一般的な原料規格内であれば許容される。かかる不純物としては例えば、水酸化カリウムに含まれるナトリウム成分、リン酸化剤の一つである無水リン酸に含まれる重金属やヒ素化合物等の各種不純物及び副生物が挙げられる。 First, the processing agent for polyester synthetic fibers according to the present invention (hereinafter referred to as the processing agent of the present invention) will be described. Examples of the alkali metal salt of an alkyl phosphate ester having an alkyl group having 12 to 22 carbon atoms in the molecule used in the treating agent of the present invention include dodecyl phosphate alkali metal salt, tridecyl phosphate alkali metal salt, and myristyl phosphate alkali. Metal salts, hexadecyl phosphate alkali metal salts, octadecyl phosphate alkali metal salts, isostearyl phosphate alkali metal salts, docosyl phosphate alkali metal salts, etc. Among them, hexadecyl phosphate alkali metal The alkyl group in the alkali metal salt of an alkyl phosphate such as a salt or octadecyl phosphate alkali metal salt is preferably one having 16 to 18 carbon atoms. These alkyl phosphate ester alkali metal salts are synthesized by a reaction between an aliphatic monohydric alcohol and a phosphorylating agent typified by anhydrous phosphoric acid, and a subsequent neutralization reaction with an alkali metal hydroxide. The aliphatic monohydric alcohol may be a single component or a mixture of two or more components. In general, an alkali metal salt of an alkyl phosphate ester is a mixture composed of a polyester containing a monoester, a diester, and a P—O—P bond, but the constituent ratio is not particularly limited. The alkali metal salt is preferably a potassium salt. About the impurity contained in a synthetic raw material, if it is in the general raw material specification, it will be accept | permitted. Examples of such impurities include a sodium component contained in potassium hydroxide and various impurities and by-products such as heavy metals and arsenic compounds contained in phosphoric anhydride which is one of phosphorylating agents.
本発明の処理剤に供するアルキルリン酸エステルのアルカリ金属塩は、その酸価が0.1〜90KOHmg/gのものであるが、なかでも0.l〜80KOHmg/gのものが好ましい。アルキルリン酸エステルのアルカリ金属塩の酸価が高すぎると、乳化不良が起こり易く、逆に酸価が0であると、繊維強度の経時低下が起こり易い。本発明において酸価とは、アルキルリン酸エステルのアルカリ金属塩をエタノール/キシレン=1/2(容量比)の混合溶媒に溶解し、電位差滴定装置にセットして、0.1mol/Lの水酸化カリウムメタノール標準溶液で滴定し、下記の数1から算出される値である。 The alkali metal salt of the alkyl phosphate ester used for the treating agent of the present invention has an acid value of 0.1 to 90 KOHmg / g, and among these, an alkali metal salt of 0. Those of 1 to 80 KOH mg / g are preferred. If the acid value of the alkali metal salt of the alkyl phosphate ester is too high, poor emulsification tends to occur, and conversely if the acid value is 0, the fiber strength tends to decrease over time. In the present invention, the acid value means that an alkali metal salt of an alkyl phosphate ester is dissolved in a mixed solvent of ethanol / xylene = 1/2 (volume ratio), set in a potentiometric titrator, and 0.1 mol / L of water. Titration with a potassium oxide methanol standard solution is a value calculated from the following formula 1.
数1において、
f:0.1mol/Lの水酸化カリウムメタノール標準溶液のファクター
S:試料採取量(g、固形分換算量)
R:変曲点までの0.1mol/Lの水酸化カリウムメタノール標準溶液の使用量(mL)
In Equation 1,
f: Factor of 0.1 mol / L potassium hydroxide methanol standard solution S: Sample collection amount (g, solid content conversion amount)
R: Amount of use of 0.1 mol / L potassium hydroxide methanol standard solution up to the inflection point (mL)
本発明の処理剤に供する界面活性剤としては、1)2−エチルヘキシルアルコール、ラウリルアルコール、ミリスチルアルコール、セチルアルコール、ステアリルアルコール、オレイルアルコール等の炭素数8〜18の飽和又は不飽和の脂肪族1価アルコールにアルキレンオキサイドを付加反応させて得られるポリオキシアルキレンアルキル(又はアルケニル)エーテル、2)カプリル酸、ラウリン酸、ミリスチン酸、パルミチン酸、ステアリン酸、オレイン酸、リノール酸、エルカ酸、リシノール酸等の炭素数8〜18の飽和又は不飽和の脂肪酸にアルキレンオキサイドを付加反応させて得られるポリオキシアルキレンアルキル(又はアルケニル)エステル、3)オクチルフェノール、ノニルフェノール等のアルキルフェノールにアルキレンオキサイドを付加反応させて得られるポリオキシアルキレンアルキルフェニルエーテル、4)オクチルアミン、ラウリルアミン、ステアリルアミン、オレイルアミン等の炭素数8〜18の飽和又は不飽和の脂肪族アミンにアルキレンオキサイドを付加反応させて得られるポリオキシアルキレンアルキル(又はアルケニル)アミノエーテル、5)前記4)のようなポリオキシアルキレンアルキル(又はアルケニル)アミノエーテルとリン酸の塩等が挙げられる。以上例示したいずれについても、ポリオキシアルキレン基としては、特に制限するものではないが、オキシアルキレン単位の数が2〜150のものが好ましく、またオキシアルキレン単位がオキシエチレン単位のみ又はオキシエチレン単位とオキシプロピレン単位とが好ましい。 As the surfactant used in the treatment agent of the present invention, 1) a saturated or unsaturated aliphatic 1 having 8 to 18 carbon atoms such as 2-ethylhexyl alcohol, lauryl alcohol, myristyl alcohol, cetyl alcohol, stearyl alcohol, oleyl alcohol, etc. Polyoxyalkylene alkyl (or alkenyl) ethers obtained by addition reaction of alkylene oxide with a hydric alcohol, 2) caprylic acid, lauric acid, myristic acid, palmitic acid, stearic acid, oleic acid, linoleic acid, erucic acid, ricinoleic acid A polyoxyalkylene alkyl (or alkenyl) ester obtained by addition reaction of an alkylene oxide with a saturated or unsaturated fatty acid having 8 to 18 carbon atoms, such as 3) an alkyl phenol such as octylphenol or nonylphenol; Polyoxyalkylene alkyl phenyl ether obtained by addition reaction of oxide, 4) Addition reaction of alkylene oxide to a saturated or unsaturated aliphatic amine having 8 to 18 carbon atoms such as octylamine, laurylamine, stearylamine, oleylamine, etc. And polyoxyalkylene alkyl (or alkenyl) amino ethers obtained as above, 5) salts of polyoxyalkylene alkyl (or alkenyl) amino ethers such as 4) and phosphoric acid, and the like. In any of the above examples, the polyoxyalkylene group is not particularly limited, but preferably has 2 to 150 oxyalkylene units, and the oxyalkylene unit is an oxyethylene unit alone or an oxyethylene unit. Oxypropylene units are preferred.
本発明の処理剤に供するリン酸金属塩は、リン酸水素二金属塩及びリン酸三金属塩から選ばれる少なくとも一つである。具体的にリン酸水素二金属塩としては、リン酸水素二カリウム塩等が挙げられ、リン酸三金属塩としては、リン酸三カリウム塩が挙げられる。なかでもリン酸金属塩としては、リン酸水素二カリウム塩等のリン酸水素二金属塩が好ましい。 The metal phosphate used for the treating agent of the present invention is at least one selected from a hydrogen phosphate dimetal salt and a phosphate trimetal salt. Specific examples of the hydrogen phosphate dimetal salt include dipotassium hydrogen phosphate, and examples of the phosphate trimetal salt include tripotassium phosphate. Among these, as the metal phosphate, a hydrogen phosphate dimetal salt such as hydrogen phosphate dipotassium salt is preferable.
本発明の処理剤は、前記した分子中に炭素数12〜22のアルキル基を有するアルキルリン酸エステルのアルカリ金属塩を40〜80質量%、前記した界面活性剤を20〜59.99質量%及び前記したリン酸金属塩を0.01〜3.0質量%(合計100質量%)の割合で含有して成るものであるが、なかでもアルキルリン酸エステルのアルカリ金属塩を40〜80質量%、界面活性剤を20〜59.99質量%及びリン酸金属塩を0.01〜1.0質量%(合計100質量%)の割合で含有して成るものが好ましく、アルキルリン酸エステルのアルカリ金属塩を50〜70質量%、界面活性剤を29.5〜49.5質量%及びリン酸金属塩を0.01〜0.50質量%(合計100質量%)の割合で含有して成るものがより好ましい。 In the treating agent of the present invention, 40-80% by mass of an alkali metal salt of an alkyl phosphate having an alkyl group having 12 to 22 carbon atoms in the molecule, and 20-59.99% by mass of the surfactant described above. And 0.01 to 3.0% by mass (total of 100% by mass) of the above-described metal phosphate, particularly 40 to 80% by weight of an alkali metal salt of an alkyl phosphate. %, A surfactant is contained in a proportion of 20 to 59.99 mass%, and a metal phosphate is contained in a proportion of 0.01 to 1.0 mass% (total 100 mass%). 50 to 70% by weight of alkali metal salt, 29.5 to 49.5% by weight of surfactant and 0.01 to 0.50% by weight (total of 100% by weight) of phosphate metal salt More preferably.
次に本発明に係るポリエステル系合成繊維の処理方法(以下、本発明の処理方法という)について説明する。本発明の処理方法は、本発明の処理剤をポリエステル系合成繊維に対し0.01〜0.5質量%となるよう付着させる方法である。付着工程は、紡糸工程、延伸工程、捲縮工程等のいずれでも良いが、紡糸工程、捲縮工程の前又は捲縮工程の後に付着させるのが好ましい。付着方法としては、浸漬給油法、スプレー給油法、ローラー給油法、計量ポンプを用いたガイド給油法等が挙げられるが、浸漬給油法、スプレー給油法又はローラー給油法が好ましい。 Next, a method for treating a polyester synthetic fiber according to the present invention (hereinafter referred to as the treatment method of the present invention) will be described. The treatment method of the present invention is a method of attaching the treatment agent of the present invention to 0.01 to 0.5% by mass with respect to the polyester-based synthetic fiber. The adhering step may be any of a spinning step, a drawing step, a crimping step, and the like, but it is preferably attached before the spinning step, the crimping step or after the crimping step. Examples of the adhesion method include an immersion oil supply method, a spray oil supply method, a roller oil supply method, a guide oil supply method using a metering pump, and the like, and an immersion oil supply method, a spray oil supply method, and a roller oil supply method are preferable.
最後に本発明に係るポリエステル系合成繊維(以下、本発明の合成繊維という)について説明する。本発明の合成繊維は、本発明の処理方法により得られるポリエステル系合成繊維である。本発明において、ポリエステル系合成繊維種としては、ポリエチレンテレフタレート繊維やポリトリメチレンテレフタレート繊維等が挙げられるが、なかでもポリエチレンテレフタレート繊維が好ましい。 Finally, the polyester synthetic fiber according to the present invention (hereinafter referred to as the synthetic fiber of the present invention) will be described. The synthetic fiber of the present invention is a polyester synthetic fiber obtained by the treatment method of the present invention. In the present invention, examples of the polyester type synthetic fiber species include polyethylene terephthalate fiber and polytrimethylene terephthalate fiber, among which polyethylene terephthalate fiber is preferable.
以上説明した本発明によると、ポリエステル系合成繊維の製造工程における延伸性不良、練条工程でのスカム堆積、加工工程での糸品位低下、更には長期在庫に伴う繊維強度の低下等を抑制できるという効果がある。 According to the present invention described above, it is possible to suppress poor stretchability in the production process of polyester-based synthetic fibers, scum accumulation in the drawing process, deterioration of yarn quality in the processing process, and further decrease in fiber strength due to long-term inventory. There is an effect.
以下、本発明の構成及び効果をより具体的にするため、実施例等を挙げるが、本発明がこれらの実施例に限定されるというものではない。尚、以下の実施例及び比較例において、部は質量部を、また%は質量%を意味する。 Hereinafter, in order to make the configuration and effects of the present invention more specific, examples and the like will be described. However, the present invention is not limited to these examples. In the following Examples and Comparative Examples, “part” means “part by mass” and “%” means “% by mass”.
試験区分1(ポリエステル系合成繊維用処理剤の5%水性液の調製)
・ポリエステル系合成繊維用処理剤(実施例1)の5%水性液の調製
オクタデシルリン酸エステルカリウム塩(酸価が10KOHmg/g)(A−1)69.5部、α−ノニルフェニル−ω−ヒドロキシ(ポリオキシエチレン)(n=10)(nはオキシエチレン単位の数、以下同じ)/α−ドデシルアミノ−ω−ヒドロキシ(ポリオキシエチレン)(n=10)=70/30(質量比)の混合物(B−1)30.0部及び燐酸水素二カリウム塩(C−1)0.5部を、80℃に加熱した所定量の半量のイオン交換水中へプロペラで撹拌下に加えて完全に溶解させた。溶解後、残りの半量のイオン交換水を一気に加えて均一になるまで撹拌し、ポリエステル系合成繊維用処理剤(実施例1)の5%水性液を調製した。
Test category 1 (Preparation of 5% aqueous solution of polyester synthetic fiber treatment agent)
-Preparation of 5% aqueous liquid of polyester synthetic fiber treating agent (Example 1) Octadecyl phosphate potassium salt (acid value is 10 KOHmg / g) (A-1) 69.5 parts, α-nonylphenyl-ω -Hydroxy (polyoxyethylene) (n = 10) (n is the number of oxyethylene units, the same applies hereinafter) / α-dodecylamino-ω-hydroxy (polyoxyethylene) (n = 10) = 70/30 (mass ratio ) 30.0 parts of the mixture (B-1) and 0.5 parts of dipotassium hydrogen phosphate (C-1) were added to a predetermined amount of half amount of ion-exchanged water heated to 80 ° C. with stirring with a propeller. It was completely dissolved. After dissolution, the remaining half of the ion-exchanged water was added all at once and stirred until uniform, to prepare a 5% aqueous liquid of a polyester synthetic fiber treating agent (Example 1).
・ポリエステル系合成繊維用処理剤(実施例2〜14及び比較例1〜8)の5%水性液の調製
ポリエステル系合成繊維用処理剤(実施例1)の5%水性液の調製と同様にして、ポリエステル系合成繊維用処理剤(実施例2〜14及び比較例1〜8)の5%水性液を調製した。各例で調製したポリエステル系合成繊維用処理剤の内容を表1にまとめて示した。
-Preparation of 5% aqueous solution of polyester-based synthetic fiber treatment agent (Examples 2-14 and Comparative Examples 1-8) Same as the preparation of 5% aqueous solution of polyester-based synthetic fiber treatment agent (Example 1) Thus, a 5% aqueous liquid of a polyester synthetic fiber treating agent (Examples 2 to 14 and Comparative Examples 1 to 8) was prepared. Table 1 summarizes the contents of the polyester synthetic fiber treating agent prepared in each example.
表1において、
A−1:オクタデシルリン酸エステルカリウム塩(酸価が10KOHmg/g)
A−2:オクタデシルリン酸エステルカリウム塩(酸価が3KOHmg/g)
A−3:オクタデシルリン酸エステルカリウム塩(酸価が90KOHmg/g)
A−4:オクタデシルリン酸エステルカリウム塩(酸価が25KOHmg/g)
A−5:セトステアリルリン酸エステルカリウム塩(酸価が5KOHmg/g)
A−6:ドデシルリン酸エステルカリウム塩(酸価が20KOHmg/g)
a−1:オクチルリン酸エステルカリウム塩(酸価が20KOHmg/g)
B−1:α−ノニルフェニル−ω−ヒドロキシ(ポリオキシエチレン)(n=10)/α−ドデシルアミノ−ω−ヒドロキシ(ポリオキシエチレン)(n=10)=70/30(質量比)の混合物
B−2:α−ドデシル−ω−ヒドロキシ(ポリオキシエチレン)(n=10)/α−ドデシル−ω−ヒドロキシ(ポリオキシエチレン)(n=5)(ポリオキシプロピレン)(m=5)/α−ドデシルアミノ−ω−ヒドロキシ(ポリオキシエチレン)(n=10)=25/25/50(質量比)の混合物(mはオキシプロピレン単位の数)
B−3:α−ドデシル−ω−ヒドロキシ(ポリオキシエチレン)(n=10)/α−ドデシルアミノ−ω−ヒドロキシ(ポリオキシエチレン)(n=10)の燐酸塩=50/50(質量比)の混合物
B−4:ヤシ脂肪酸−ポリオキシエチレン(n=10)/α−ドデシルアミノ−ω−ヒドロキシ(ポリオキシエチレン)(n=10)=50/50(質量比)の混合物
b−1:ポリエチレングリコール(数平均分子量が1000)
C−1:燐酸水素二カリウム塩
C−2:燐酸三カリウム塩
In Table 1,
A-1: Potassium salt of octadecyl phosphate (acid value is 10 KOHmg / g)
A-2: Octadecyl phosphate potassium salt (acid value is 3 KOHmg / g)
A-3: Octadecyl phosphate potassium salt (acid value is 90 KOHmg / g)
A-4: Octadecyl phosphate potassium salt (acid value is 25 KOHmg / g)
A-5: Cetostearyl phosphate potassium salt (acid value is 5 KOHmg / g)
A-6: Dodecyl phosphate potassium salt (acid value is 20 KOHmg / g)
a-1: Octyl phosphate ester potassium salt (acid value is 20 KOHmg / g)
B-1: α-nonylphenyl-ω-hydroxy (polyoxyethylene) (n = 10) / α-dodecylamino-ω-hydroxy (polyoxyethylene) (n = 10) = 70/30 (mass ratio) Mixture B-2: α-dodecyl-ω-hydroxy (polyoxyethylene) (n = 10) / α-dodecyl-ω-hydroxy (polyoxyethylene) (n = 5) (polyoxypropylene) (m = 5) / Α-dodecylamino-ω-hydroxy (polyoxyethylene) (n = 10) = 25/25/50 (mass ratio) mixture (m is the number of oxypropylene units)
B-3: α-dodecyl-ω-hydroxy (polyoxyethylene) (n = 10) / α-dodecylamino-ω-hydroxy (polyoxyethylene) (n = 10) phosphate = 50/50 (mass ratio) ) B-4: Mixture of coconut fatty acid-polyoxyethylene (n = 10) / α-dodecylamino-ω-hydroxy (polyoxyethylene) (n = 10) = 50/50 (mass ratio) b-1 : Polyethylene glycol (number average molecular weight is 1000)
C-1: Dipotassium hydrogen phosphate C-2: Tripotassium phosphate
試験区分2(ポリエステル系合成繊維用処理剤の5%水性液の安定性の評価)
試験区分1で調製した各例のポリエステル系合成繊維用処理剤の5%水性液について、肉眼観察によりその安定性を下記の基準で評価した。結果を表2にまとめて示した。
Test category 2 (Evaluation of stability of 5% aqueous liquid of polyester synthetic fiber treatment agent)
The stability of the 5% aqueous liquid of the polyester synthetic fiber treating agent of each example prepared in Test Category 1 was evaluated by visual observation according to the following criteria. The results are summarized in Table 2.
安定性の評価基準
○○○:全く潤みがなく、安定性極めて良好
○○:僅かに潤みはあるが、安定性良好
○:少し潤みはあるが、全体として安定性良好
×:沈殿及び浮遊物が発生しており、安定性不良
Evaluation criteria for stability XX: No moisture at all, very good stability XX: Slightly moistened, but good stability ◯: Slightly moistened, but overall stable X: Precipitation and suspended matter Has occurred and the stability is poor
試験区分3(ポリエステルステープル繊維への処理剤の付着とその評価)
・ポリエステルステープル繊維への処理剤の付着
試験区分1で調製したポリエステル系合成繊維用処理剤の5%水性液を水希釈して2%水性液とした。この2%水性液を、製綿工程で得られた繊度1.3×10−4g/m(1.2デニール)で繊維長38mmのセミダルのポリエステルステープル繊維に、付着量が0.15%となるようスプレー給油法で付着させ、80℃の熱風乾燥機で2時間乾燥した後、25℃×40%RHの雰囲気下に一夜調湿して、ポリエステル系合成繊維用処理剤を付着させた処理済みポリエステルステープル繊維を得た。
Test Category 3 (Attachment of treatment agent to polyester staple fiber and its evaluation)
-Adhesion of treatment agent to polyester staple fiber A 5% aqueous solution of the polyester synthetic fiber treatment agent prepared in Test Category 1 was diluted with water to give a 2% aqueous solution. This 2% aqueous liquid was attached to a semi-dal polyester staple fiber having a fineness of 1.3 × 10 −4 g / m (1.2 denier) and a fiber length of 38 mm obtained in the cotton-making process, and the adhesion amount was 0.15%. After being dried by a spray oiling method and dried with a hot air dryer at 80 ° C. for 2 hours, the moisture was conditioned overnight in an atmosphere of 25 ° C. × 40% RH to adhere a polyester synthetic fiber treatment agent. A treated polyester staple fiber was obtained.
・練条工程での耐スカム堆積性の評価
前記の処理済みポリエステルステープル繊維10kgを用い、フラットカード(豊和工業社製)に供してカードスライバーを得た。得られたカードスライバーを、30℃で70%RHの雰囲気下にPDF型練条機(石川製作所社製)に供し、紡出速度=250m/分の条件で5回繰り返して通過させた。PDF型練条機のゴムローラー、レジューサー及びトランペットの各部分におけるスカムの程度を以下の基準で肉眼判定した。結果を表2にまとめて示した。
-Evaluation of scum accumulation resistance in the drawing step Using 10 kg of the treated polyester staple fiber, it was subjected to a flat card (manufactured by Toyoka Industries Co., Ltd.) to obtain a card sliver. The obtained card sliver was subjected to a PDF type drawing machine (manufactured by Ishikawa Seisakusho) in an atmosphere of 70% RH at 30 ° C. and repeatedly passed 5 times under the condition of spinning speed = 250 m / min. The degree of scum in each part of the rubber roller, reducer, and trumpet of the PDF type drawing machine was determined with the following criteria. The results are summarized in Table 2.
耐スカム堆積性の評価基準
○○○:全くスカムの堆積が認められない
○○:僅かにスカムの堆積が認められるが、問題ない
○:少しスカムの堆積が認められるが、全体として問題ない
×:明らかにスカムの堆積が認められ、スライバー巻きつきが生じ、問題がある
Evaluation criteria for resistance to scum accumulation ○○○: No scum accumulation is observed ○○: Scum accumulation is observed slightly, but no problem ○: Scum accumulation is observed slightly, but there is no problem as a whole × : Clearly scum accumulation, sliver wrapping, causing problems
・糸品位の評価
前記の処理済みポリエステルステープル繊維10kgを用い、フラットカード(豊和工業社製)に供してカードスライバーを得た。得られたカードスライバーをPDF型練条機(石川製作所製)及び粗紡機(豊田自動織機社製)に供して粗糸を得た。得られた粗糸をリング精紡機(豊田自動織機社製)に供し、スピンドル回転数=20000rpm、撚り数775T/m、供給粗糸=0.59g/m、トータルドラフト=40倍の条件で2時間、20錘で運転し、アンチノードリングへの白粉堆積を肉眼観察して、糸品位を以下の基準で評価した。結果を表2にまとめて示した。
-Evaluation of yarn quality Using 10 kg of the above treated polyester staple fiber, it was subjected to a flat card (manufactured by Toyoka Industries Co., Ltd.) to obtain a card sliver. The obtained card sliver was subjected to a PDF type drawing machine (manufactured by Ishikawa Seisakusho) and a roving machine (manufactured by Toyota Industries Corporation) to obtain a roving yarn. The obtained roving yarn is supplied to a ring spinning machine (manufactured by Toyota Industries Corporation). The operation was performed for 20 spindles for a time, and white powder accumulation on the anti-node ring was observed with naked eyes, and the yarn quality was evaluated according to the following criteria. The results are summarized in Table 2.
糸品位の評価基準
○○○:白粉堆積が認められず、繊維損傷も殆ど無く、糸品位は極めて良好
○○:僅かに白粉堆積が認められ、僅かに繊維損傷があるが、糸品位は良好
○:少し白粉堆積が認められ、少しの繊維損傷があるが、全体として糸品位は良好
×:白粉堆積が多く認められ、繊維損傷も多く認められて、糸品位は不良
Evaluation criteria for yarn quality ○○○: No white powder accumulation, almost no fiber damage, very good yarn quality ○○: Slight white powder accumulation, slight fiber damage, but good yarn quality ○: Slight white powder accumulation is observed and there is slight fiber damage, but the yarn quality as a whole is good. ×: Many white powder accumulation is observed, and many fiber damage is observed, resulting in poor yarn quality.
・繊維強度の評価
前記の処理済みポリエステルステープル繊維について、初期強度と、30℃で70%RHの雰囲気下に3カ月間保管した後の強度を強伸度測定機にて測定した。3カ月後の強度を初期強度比較することにより、繊維強度を以下の基準で評価した。結果を表1にまとめて示した。
-Evaluation of fiber strength About the said processed polyester staple fiber, the initial strength and the intensity | strength after storing for 3 months in the atmosphere of 70% RH at 30 degreeC were measured with the strong elongation measuring machine. By comparing the strength after 3 months with the initial strength, the fiber strength was evaluated according to the following criteria. The results are summarized in Table 1.
繊維強度の評価基準
○○○:初期強度に対して98%以上の強度
○○:初期強度に対して97%以上98%未満の強度
○:初期強度に対して95%以上97%未満の強度
×:初期強度に対して95%未満の強度
Evaluation criteria for fiber strength XX: Strength of 98% or more with respect to initial strength XX: Strength of 97% or more and less than 98% with respect to initial strength ◯: Strength of 95% or more and less than 97% with respect to initial strength X: Strength less than 95% of initial strength
・延伸性の評価
試験区分1で調製したポリエステル系合成繊維用処理剤の5%水性液を水希釈して1%水性液とした。離間して軸受した上流側のフリーローラと下流側のフリーローラとの間に、容器に収容した円筒状の摩擦体を配置し、容器内に前記の1%水性液を満たした。脱脂したポリエステルフィラメント(120デニール/36フィラメント)を、上流側のフリーローラと下流側のフリーローラとでガイドしつつ、1%水性液に完全に浸した摩擦体に接触させ、低速ワインダーにより50m/分の速度で引っ張った。このときの上流側のフリーローラの直前の張力T1と、下流側のフリーローラの直後の張力T2を求め、T2/T1を算出し、延伸性を下記の基準で評価した。結果を表2にまとめて示した。
-Evaluation of stretchability A 5% aqueous liquid of the polyester synthetic fiber treating agent prepared in Test Category 1 was diluted with water to obtain a 1% aqueous liquid. A cylindrical friction body accommodated in a container was disposed between the free roller on the upstream side and the free roller on the downstream side that were spaced apart from each other, and the container was filled with the 1% aqueous liquid. The degreased polyester filament (120 denier / 36 filament) is guided by an upstream free roller and a downstream free roller, and brought into contact with a friction body completely immersed in a 1% aqueous liquid, and 50 m / m by a low speed winder. Pulled at a speed of minutes. At this time, the tension T1 immediately before the upstream free roller and the tension T2 immediately after the downstream free roller were determined, T2 / T1 was calculated, and the stretchability was evaluated according to the following criteria. The results are summarized in Table 2.
延伸性の評価基準
○○○:T2/T1=6.00未満
○○:T2/T1=6.00以上6.10未満
○:T2/T1=6.10以上6.30未満
×:T2/T1=6.30以上
Evaluation criteria for stretchability OO: T2 / T1 = less than 6.00 OO: T2 / T1 = 6.00 or more and less than 6.10 O: T2 / T1 = 6.00 or more and less than 6.30 X: T2 / T1 = 6.30 or more
表1に対応する表2の結果からも明らかなように、本発明によれば、ポリエステル系合成繊維の製造工程における延伸性不良、練条工程でのスカム堆積、加工工程での糸品位低下、更には長期在庫に伴う繊維強度の低下等を抑制できるという効果がある。 As is apparent from the results of Table 2 corresponding to Table 1, according to the present invention, poor stretchability in the production process of the polyester-based synthetic fiber, scum deposition in the drawing process, and yarn quality deterioration in the processing process, Furthermore, there is an effect that it is possible to suppress a decrease in fiber strength associated with long-term inventory.
Claims (10)
界面活性剤:ポリオキシアルキレンアルキルエーテル、ポリオキシアルキレンアルケニルエーテル、ポリオキシアルキレンアルキルエステル、ポリオキシアルキレンアルケニルエステル、ポリオキシアルキレンアルキルフェニルエーテル、ポリオキシアルキレンアルキルアミノエーテル、ポリオキシアルキレンアルケニルアミノエーテル、ポリオキシアルキレンアルキルアミノエーテルと無機酸との塩及びポリオキシアルキレンアルケニルアミノエーテルと無機酸との塩から選ばれる少なくとも一つ
リン酸金属塩:リン酸水素二金属塩及びリン酸三金属塩から選ばれる少なくとも一つ 40-80% by mass of an alkali metal salt of an alkyl phosphate having an alkyl group having 12 to 22 carbon atoms in the molecule, 20-59.9% by mass of the following surfactant, and 0 of the following metal phosphate A polyester system characterized by comprising 0.01 to 3.0% by mass (100% by mass in total), wherein the alkali metal salt of the alkyl phosphate ester has an acid value of 0.1 to 90 KOHmg / g Treatment agent for synthetic fibers.
Surfactant: polyoxyalkylene alkyl ether, polyoxyalkylene alkenyl ether, polyoxyalkylene alkyl ester, polyoxyalkylene alkenyl ester, polyoxyalkylene alkyl phenyl ether, polyoxyalkylene alkyl amino ether, polyoxyalkylene alkenyl amino ether, poly At least one selected from a salt of an oxyalkylene alkylamino ether and an inorganic acid and a salt of a polyoxyalkylene alkenyl amino ether and an inorganic acid. Phosphorus metal salt: selected from a bimetallic hydrogen phosphate and a trimetallic phosphate At least one
Priority Applications (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP2015104031A JP5796922B1 (en) | 2015-05-21 | 2015-05-21 | Polyester synthetic fiber treatment agent, polyester synthetic fiber treatment method, and polyester synthetic fiber |
CN201610185116.6A CN106167986B (en) | 2015-05-21 | 2016-03-29 | Treating agent for polyester synthetic fiber, method for treating polyester synthetic fiber, and polyester synthetic fiber |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP2015104031A JP5796922B1 (en) | 2015-05-21 | 2015-05-21 | Polyester synthetic fiber treatment agent, polyester synthetic fiber treatment method, and polyester synthetic fiber |
Publications (2)
Publication Number | Publication Date |
---|---|
JP5796922B1 true JP5796922B1 (en) | 2015-10-21 |
JP2016216858A JP2016216858A (en) | 2016-12-22 |
Family
ID=54348590
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
JP2015104031A Active JP5796922B1 (en) | 2015-05-21 | 2015-05-21 | Polyester synthetic fiber treatment agent, polyester synthetic fiber treatment method, and polyester synthetic fiber |
Country Status (2)
Country | Link |
---|---|
JP (1) | JP5796922B1 (en) |
CN (1) | CN106167986B (en) |
Families Citing this family (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP6348246B1 (en) * | 2017-04-18 | 2018-06-27 | 竹本油脂株式会社 | Treatment agent for polyester synthetic fiber and polyester synthetic fiber |
WO2019239597A1 (en) * | 2018-06-15 | 2019-12-19 | 竹本油脂株式会社 | Polyester synthetic fiber treatment agent and polyester synthetic fibers |
US11359309B2 (en) | 2018-12-21 | 2022-06-14 | Target Brands, Inc. | Ring spun yarn and method |
Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS53103099A (en) * | 1977-02-22 | 1978-09-07 | Takemoto Oil & Fat Co Ltd | Novel oil agent for treating synthetic fiber |
JPS53106896A (en) * | 1977-02-22 | 1978-09-18 | Toyo Boseki | Antistatic finish of polyester fiber being able to be dyed by ionic dyestuff |
Family Cites Families (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP3222215B2 (en) * | 1992-09-24 | 2001-10-22 | 松本油脂製薬株式会社 | Oil agent for polyester fiber processing for spinning |
JP4691429B2 (en) * | 2005-10-13 | 2011-06-01 | 竹本油脂株式会社 | Synthetic fiber treatment agent and method for manufacturing nonwoven fabric and nonwoven fabric manufacturing fabric |
JP4480176B2 (en) * | 2006-12-27 | 2010-06-16 | 竹本油脂株式会社 | Synthetic fiber treatment liquid and synthetic fiber treatment method |
-
2015
- 2015-05-21 JP JP2015104031A patent/JP5796922B1/en active Active
-
2016
- 2016-03-29 CN CN201610185116.6A patent/CN106167986B/en active Active
Patent Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS53103099A (en) * | 1977-02-22 | 1978-09-07 | Takemoto Oil & Fat Co Ltd | Novel oil agent for treating synthetic fiber |
JPS53106896A (en) * | 1977-02-22 | 1978-09-18 | Toyo Boseki | Antistatic finish of polyester fiber being able to be dyed by ionic dyestuff |
Also Published As
Publication number | Publication date |
---|---|
CN106167986B (en) | 2017-10-27 |
JP2016216858A (en) | 2016-12-22 |
CN106167986A (en) | 2016-11-30 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
JP5796922B1 (en) | Polyester synthetic fiber treatment agent, polyester synthetic fiber treatment method, and polyester synthetic fiber | |
JP6962618B1 (en) | Elastic fiber treatment agent and elastic fiber | |
JP5796921B1 (en) | Polyester synthetic fiber spinning treatment, polyester synthetic fiber treatment method and polyester synthetic fiber | |
CN106192393B (en) | Treating agent for polyester synthetic fiber, method for treating polyester synthetic fiber, and polyester synthetic fiber | |
JP4471464B2 (en) | Oil for high-speed spinning of synthetic fiber and high-speed spinning method | |
US20230349096A1 (en) | Elastic fiber treating agent and elastic fibers | |
JP6348246B1 (en) | Treatment agent for polyester synthetic fiber and polyester synthetic fiber | |
JP2009138282A (en) | Treating agent for elastic fibers and elastic fibers | |
WO2023282285A1 (en) | Treatment agent for fibers, first treatment agent for fibers, second treatment agent for fibers, composition containing first treatment agent for fibers, diluent for treatment agent for fibers, treatment method for fibers, and fibers | |
CN111684124B (en) | Treating agent for polyester synthetic fiber and polyester synthetic fiber | |
KR102689018B1 (en) | Treatment agent for staple fibers, aqueous solution of treatment agent for staple fibers, method for treating staple fibers, method for producing staple fibers, and staple fibers | |
JPWO2009098845A1 (en) | Fiber treatment agent and method for producing synthetic fiber | |
JP4471463B2 (en) | Oil for high-speed spinning of synthetic fiber and high-speed spinning method | |
JP5588229B2 (en) | Fiber treatment agent and method for producing synthetic fiber | |
US3245905A (en) | Blended fibers having improved antistatic properties | |
JP2021014644A (en) | Elastic fiber treatment agent and elastic fiber | |
JP6967815B1 (en) | Synthetic fiber treatment agent, synthetic fiber and synthetic fiber treatment method | |
WO2023080023A1 (en) | Composition containing first treatment agent for synthetic fiber, method for preparing diluted solution of treatment agent for synthetic fiber, method for treating synthetic fiber, method for producing synthetic fiber, and method for producing short fiber | |
JP2023107721A (en) | Treating agent for elastic fibers and elastic fibers | |
WO2021251283A1 (en) | Synthetic fiber treatment agent and synthetic fibers | |
JP2004360083A (en) | Synthetic fiber-treating agent and method for treating synthetic fiber | |
JP2004360082A (en) | Synthetic fiber-treating agent and method for treating synthetic fiber |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
TRDD | Decision of grant or rejection written | ||
A975 | Report on accelerated examination |
Free format text: JAPANESE INTERMEDIATE CODE: A971005 Effective date: 20150807 |
|
A01 | Written decision to grant a patent or to grant a registration (utility model) |
Free format text: JAPANESE INTERMEDIATE CODE: A01 Effective date: 20150817 |
|
A61 | First payment of annual fees (during grant procedure) |
Free format text: JAPANESE INTERMEDIATE CODE: A61 Effective date: 20150817 |
|
R150 | Certificate of patent or registration of utility model |
Ref document number: 5796922 Country of ref document: JP Free format text: JAPANESE INTERMEDIATE CODE: R150 |
|
R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |