JP5399859B2 - Method for producing polyphenol processed fiber - Google Patents
Method for producing polyphenol processed fiber Download PDFInfo
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- JP5399859B2 JP5399859B2 JP2009246391A JP2009246391A JP5399859B2 JP 5399859 B2 JP5399859 B2 JP 5399859B2 JP 2009246391 A JP2009246391 A JP 2009246391A JP 2009246391 A JP2009246391 A JP 2009246391A JP 5399859 B2 JP5399859 B2 JP 5399859B2
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- Prior art keywords
- polyphenol
- fiber
- water
- cotton fabric
- fastness
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- 235000013824 polyphenols Nutrition 0.000 title claims description 169
- 150000008442 polyphenolic compounds Chemical class 0.000 title claims description 162
- 239000000835 fiber Substances 0.000 title claims description 110
- 238000004519 manufacturing process Methods 0.000 title claims description 13
- -1 phenylamide compound Chemical class 0.000 claims description 24
- 238000000034 method Methods 0.000 claims description 22
- 125000000129 anionic group Chemical group 0.000 claims description 14
- 239000007788 liquid Substances 0.000 claims description 14
- 150000001450 anions Chemical class 0.000 claims description 12
- 229920000642 polymer Polymers 0.000 claims description 10
- 239000006185 dispersion Substances 0.000 claims description 8
- 244000269722 Thea sinensis Species 0.000 claims description 5
- 235000009754 Vitis X bourquina Nutrition 0.000 claims description 4
- 235000012333 Vitis X labruscana Nutrition 0.000 claims description 4
- 240000006365 Vitis vinifera Species 0.000 claims description 4
- 235000014787 Vitis vinifera Nutrition 0.000 claims description 4
- 230000008569 process Effects 0.000 claims description 4
- 239000004744 fabric Substances 0.000 description 114
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 104
- 229920000742 Cotton Polymers 0.000 description 91
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 74
- 239000000460 chlorine Substances 0.000 description 73
- 229910052801 chlorine Inorganic materials 0.000 description 73
- 239000003795 chemical substances by application Substances 0.000 description 54
- 238000004043 dyeing Methods 0.000 description 34
- KXDAEFPNCMNJSK-UHFFFAOYSA-N Benzamide Chemical compound NC(=O)C1=CC=CC=C1 KXDAEFPNCMNJSK-UHFFFAOYSA-N 0.000 description 27
- 238000012545 processing Methods 0.000 description 23
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 21
- 230000002378 acidificating effect Effects 0.000 description 16
- 238000003756 stirring Methods 0.000 description 16
- 239000000243 solution Substances 0.000 description 15
- 239000007864 aqueous solution Substances 0.000 description 13
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- 238000005406 washing Methods 0.000 description 13
- 239000000047 product Substances 0.000 description 12
- 241000196324 Embryophyta Species 0.000 description 11
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- 239000004677 Nylon Substances 0.000 description 10
- 238000004061 bleaching Methods 0.000 description 9
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 9
- 238000007670 refining Methods 0.000 description 9
- 239000011347 resin Substances 0.000 description 9
- 229920005989 resin Polymers 0.000 description 9
- TVQLLNFANZSCGY-UHFFFAOYSA-N disodium;dioxido(oxo)tin Chemical compound [Na+].[Na+].[O-][Sn]([O-])=O TVQLLNFANZSCGY-UHFFFAOYSA-N 0.000 description 8
- 229940079864 sodium stannate Drugs 0.000 description 8
- 239000000126 substance Substances 0.000 description 8
- 230000000844 anti-bacterial effect Effects 0.000 description 7
- 230000008859 change Effects 0.000 description 7
- 238000011161 development Methods 0.000 description 7
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- 230000003078 antioxidant effect Effects 0.000 description 6
- 238000006243 chemical reaction Methods 0.000 description 6
- 238000002845 discoloration Methods 0.000 description 6
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N phenol group Chemical group C1(=CC=CC=C1)O ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 6
- 235000013616 tea Nutrition 0.000 description 6
- 125000002091 cationic group Chemical group 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical group NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 description 4
- 241000894006 Bacteria Species 0.000 description 4
- 230000006872 improvement Effects 0.000 description 4
- 125000001424 substituent group Chemical group 0.000 description 4
- 229920001864 tannin Polymers 0.000 description 4
- 235000018553 tannin Nutrition 0.000 description 4
- 239000001648 tannin Substances 0.000 description 4
- 239000004753 textile Substances 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- 229920000178 Acrylic resin Polymers 0.000 description 3
- 239000004925 Acrylic resin Substances 0.000 description 3
- 239000002253 acid Substances 0.000 description 3
- 230000003385 bacteriostatic effect Effects 0.000 description 3
- 150000001768 cations Chemical class 0.000 description 3
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- 238000007922 dissolution test Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
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- 230000007246 mechanism Effects 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 230000001590 oxidative effect Effects 0.000 description 3
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 3
- 150000003242 quaternary ammonium salts Chemical class 0.000 description 3
- 230000027756 respiratory electron transport chain Effects 0.000 description 3
- 210000004243 sweat Anatomy 0.000 description 3
- VVJKKWFAADXIJK-UHFFFAOYSA-N Allylamine Chemical compound NCC=C VVJKKWFAADXIJK-UHFFFAOYSA-N 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 2
- 241000219094 Vitaceae Species 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 125000003368 amide group Chemical group 0.000 description 2
- 239000003963 antioxidant agent Substances 0.000 description 2
- 235000006708 antioxidants Nutrition 0.000 description 2
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 2
- 238000011109 contamination Methods 0.000 description 2
- 125000004122 cyclic group Chemical group 0.000 description 2
- 230000001877 deodorizing effect Effects 0.000 description 2
- 239000004815 dispersion polymer Substances 0.000 description 2
- 239000000839 emulsion Substances 0.000 description 2
- 235000019225 fermented tea Nutrition 0.000 description 2
- 235000021021 grapes Nutrition 0.000 description 2
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 2
- ZQEIXNIJLIKNTD-UHFFFAOYSA-N methyl N-(2,6-dimethylphenyl)-N-(methoxyacetyl)alaninate Chemical compound COCC(=O)N(C(C)C(=O)OC)C1=C(C)C=CC=C1C ZQEIXNIJLIKNTD-UHFFFAOYSA-N 0.000 description 2
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 125000004433 nitrogen atom Chemical group N* 0.000 description 2
- 239000000575 pesticide Substances 0.000 description 2
- 230000000704 physical effect Effects 0.000 description 2
- 239000008399 tap water Substances 0.000 description 2
- 235000020679 tap water Nutrition 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- TUSDEZXZIZRFGC-UHFFFAOYSA-N 1-O-galloyl-3,6-(R)-HHDP-beta-D-glucose Natural products OC1C(O2)COC(=O)C3=CC(O)=C(O)C(O)=C3C3=C(O)C(O)=C(O)C=C3C(=O)OC1C(O)C2OC(=O)C1=CC(O)=C(O)C(O)=C1 TUSDEZXZIZRFGC-UHFFFAOYSA-N 0.000 description 1
- XYHKNCXZYYTLRG-UHFFFAOYSA-N 1h-imidazole-2-carbaldehyde Chemical compound O=CC1=NC=CN1 XYHKNCXZYYTLRG-UHFFFAOYSA-N 0.000 description 1
- GWYFCOCPABKNJV-UHFFFAOYSA-M 3-Methylbutanoic acid Natural products CC(C)CC([O-])=O GWYFCOCPABKNJV-UHFFFAOYSA-M 0.000 description 1
- 229920002972 Acrylic fiber Polymers 0.000 description 1
- 239000005734 Benalaxyl Substances 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 235000014036 Castanea Nutrition 0.000 description 1
- 241001070941 Castanea Species 0.000 description 1
- 229920003043 Cellulose fiber Polymers 0.000 description 1
- 244000223760 Cinnamomum zeylanicum Species 0.000 description 1
- 240000007154 Coffea arabica Species 0.000 description 1
- 244000061508 Eriobotrya japonica Species 0.000 description 1
- 235000009008 Eriobotrya japonica Nutrition 0.000 description 1
- 239000001263 FEMA 3042 Substances 0.000 description 1
- 240000008620 Fagopyrum esculentum Species 0.000 description 1
- 235000009419 Fagopyrum esculentum Nutrition 0.000 description 1
- 240000009088 Fragaria x ananassa Species 0.000 description 1
- OYHQOLUKZRVURQ-HZJYTTRNSA-N Linoleic acid Chemical compound CCCCC\C=C/C\C=C/CCCCCCCC(O)=O OYHQOLUKZRVURQ-HZJYTTRNSA-N 0.000 description 1
- 244000070406 Malus silvestris Species 0.000 description 1
- 239000005807 Metalaxyl Substances 0.000 description 1
- 241001465754 Metazoa Species 0.000 description 1
- YXOLAZRVSSWPPT-UHFFFAOYSA-N Morin Chemical compound OC1=CC(O)=CC=C1C1=C(O)C(=O)C2=C(O)C=C(O)C=C2O1 YXOLAZRVSSWPPT-UHFFFAOYSA-N 0.000 description 1
- CHJJGSNFBQVOTG-UHFFFAOYSA-N N-methyl-guanidine Natural products CNC(N)=N CHJJGSNFBQVOTG-UHFFFAOYSA-N 0.000 description 1
- 239000006057 Non-nutritive feed additive Substances 0.000 description 1
- 241000207836 Olea <angiosperm> Species 0.000 description 1
- LRBQNJMCXXYXIU-PPKXGCFTSA-N Penta-digallate-beta-D-glucose Natural products OC1=C(O)C(O)=CC(C(=O)OC=2C(=C(O)C=C(C=2)C(=O)OC[C@@H]2[C@H]([C@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)O2)OC(=O)C=2C=C(OC(=O)C=3C=C(O)C(O)=C(O)C=3)C(O)=C(O)C=2)O)=C1 LRBQNJMCXXYXIU-PPKXGCFTSA-N 0.000 description 1
- 235000004347 Perilla Nutrition 0.000 description 1
- 244000124853 Perilla frutescens Species 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical group OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
- 108010039918 Polylysine Proteins 0.000 description 1
- 239000004743 Polypropylene Substances 0.000 description 1
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- 244000294611 Punica granatum Species 0.000 description 1
- 235000014360 Punica granatum Nutrition 0.000 description 1
- 229920000297 Rayon Polymers 0.000 description 1
- 241000220317 Rosa Species 0.000 description 1
- 241000191967 Staphylococcus aureus Species 0.000 description 1
- 240000001417 Vigna umbellata Species 0.000 description 1
- 235000011453 Vigna umbellata Nutrition 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 229920006221 acetate fiber Polymers 0.000 description 1
- 229920006243 acrylic copolymer Polymers 0.000 description 1
- 125000001931 aliphatic group Chemical group 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- ZRALSGWEFCBTJO-UHFFFAOYSA-N anhydrous guanidine Natural products NC(N)=N ZRALSGWEFCBTJO-UHFFFAOYSA-N 0.000 description 1
- 229920006318 anionic polymer Polymers 0.000 description 1
- 239000003242 anti bacterial agent Substances 0.000 description 1
- 235000021016 apples Nutrition 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 235000021028 berry Nutrition 0.000 description 1
- GWYFCOCPABKNJV-UHFFFAOYSA-N beta-methyl-butyric acid Natural products CC(C)CC(O)=O GWYFCOCPABKNJV-UHFFFAOYSA-N 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 239000004202 carbamide Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 125000002843 carboxylic acid group Chemical group 0.000 description 1
- 150000001765 catechin Chemical class 0.000 description 1
- ADRVNXBAWSRFAJ-UHFFFAOYSA-N catechin Natural products OC1Cc2cc(O)cc(O)c2OC1c3ccc(O)c(O)c3 ADRVNXBAWSRFAJ-UHFFFAOYSA-N 0.000 description 1
- 235000005487 catechin Nutrition 0.000 description 1
- 229920006317 cationic polymer Polymers 0.000 description 1
- 238000004587 chromatography analysis Methods 0.000 description 1
- 235000017803 cinnamon Nutrition 0.000 description 1
- 230000015271 coagulation Effects 0.000 description 1
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- 235000016213 coffee Nutrition 0.000 description 1
- 235000013353 coffee beverage Nutrition 0.000 description 1
- 238000004042 decolorization Methods 0.000 description 1
- 239000007933 dermal patch Substances 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 150000004985 diamines Chemical class 0.000 description 1
- VILAVOFMIJHSJA-UHFFFAOYSA-N dicarbon monoxide Chemical group [C]=C=O VILAVOFMIJHSJA-UHFFFAOYSA-N 0.000 description 1
- SWSQBOPZIKWTGO-UHFFFAOYSA-N dimethylaminoamidine Natural products CN(C)C(N)=N SWSQBOPZIKWTGO-UHFFFAOYSA-N 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- RTZKZFJDLAIYFH-UHFFFAOYSA-N ether Substances CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 238000005562 fading Methods 0.000 description 1
- 238000005187 foaming Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 125000005843 halogen group Chemical group 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
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- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 238000011081 inoculation Methods 0.000 description 1
- OYHQOLUKZRVURQ-IXWMQOLASA-N linoleic acid Natural products CCCCC\C=C/C\C=C\CCCCCCCC(O)=O OYHQOLUKZRVURQ-IXWMQOLASA-N 0.000 description 1
- 235000020778 linoleic acid Nutrition 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- CJPQIRJHIZUAQP-UHFFFAOYSA-N methyl N-(2,6-dimethylphenyl)-N-(phenylacetyl)alaninate Chemical compound CC=1C=CC=C(C)C=1N(C(C)C(=O)OC)C(=O)CC1=CC=CC=C1 CJPQIRJHIZUAQP-UHFFFAOYSA-N 0.000 description 1
- CIEXPHRYOLIQQD-UHFFFAOYSA-N methyl N-(2,6-dimethylphenyl)-N-2-furoylalaninate Chemical compound CC=1C=CC=C(C)C=1N(C(C)C(=O)OC)C(=O)C1=CC=CO1 CIEXPHRYOLIQQD-UHFFFAOYSA-N 0.000 description 1
- UXOUKMQIEVGVLY-UHFFFAOYSA-N morin Natural products OC1=CC(O)=CC(C2=C(C(=O)C3=C(O)C=C(O)C=C3O2)O)=C1 UXOUKMQIEVGVLY-UHFFFAOYSA-N 0.000 description 1
- 235000007708 morin Nutrition 0.000 description 1
- QOGAQGLPMQVRTR-UHFFFAOYSA-N n-(3-chlorophenyl)cyclopropanecarboxamide Chemical compound ClC1=CC=CC(NC(=O)C2CC2)=C1 QOGAQGLPMQVRTR-UHFFFAOYSA-N 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- UWVQIROCRJWDKL-UHFFFAOYSA-N oxadixyl Chemical compound CC=1C=CC=C(C)C=1N(C(=O)COC)N1CCOC1=O UWVQIROCRJWDKL-UHFFFAOYSA-N 0.000 description 1
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- 125000002467 phosphate group Chemical group [H]OP(=O)(O[H])O[*] 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 229920000747 poly(lactic acid) Polymers 0.000 description 1
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- 235000021012 strawberries Nutrition 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
- LRBQNJMCXXYXIU-NRMVVENXSA-N tannic acid Chemical compound OC1=C(O)C(O)=CC(C(=O)OC=2C(=C(O)C=C(C=2)C(=O)OC[C@@H]2[C@H]([C@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)O2)OC(=O)C=2C=C(OC(=O)C=3C=C(O)C(O)=C(O)C=3)C(O)=C(O)C=2)O)=C1 LRBQNJMCXXYXIU-NRMVVENXSA-N 0.000 description 1
- 229940033123 tannic acid Drugs 0.000 description 1
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- 229920002258 tannic acid Polymers 0.000 description 1
- 150000003585 thioureas Chemical class 0.000 description 1
Landscapes
- Coloring (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
Description
本発明は、植物等に含まれる天然成分であるポリフェノール化合物を用いた染色によって堅牢度の高い染め色を繊維に付与可能なポリフェノール加工繊維の製造方法に関し、特に、水処理剤等に起因する塩素を含有する水道水で洗浄しても良好な染め色を保つことができる塩素堅牢度を備えたポリフェノール加工繊維の製造方法に関する。 The present invention relates to a method for producing a polyphenol-processed fiber that can impart to a fiber a dyed color with high fastness by dyeing using a polyphenol compound that is a natural component contained in plants, and in particular, chlorine caused by a water treatment agent or the like. The present invention relates to a method for producing a polyphenol-processed fiber having a chlorine fastness capable of maintaining a good dyed color even when washed with contained tap water.
植物等に含まれるポリフェノール化合物は、天然色素として、古来より伝わる伝統的な草木染めに用いられる。また、近年、ポリフェノールを繊維に固着させてその機能性（抗菌性等）を繊維に付与する加工技術が開発され、1)バインダー樹脂によるパディング加工法、2)工業用金属塩を用いた金属媒染法、3)カチオン高分子等を用いた浸染的手法などの技術がある。このような草木染め技術やポリフェノール加工においては、発色又は機能性を保持しながら染色堅牢度を維持することが商品化及び広範な普及のための必須条件であるので、工業化においては、発色そのものを向上させる技術及び機能を発現させる技術において進歩が見られる。 Polyphenol compounds contained in plants and the like are used as natural pigments in traditional plant dyeing that has been passed down since ancient times. In recent years, processing technology has been developed to fix polyphenols to fibers and impart their functionality (antibacterial properties, etc.) to the fibers. 1) Padding process using binder resin, 2) Metal mordanting using industrial metal salts 3) Technology such as dip dyeing using cationic polymers. In such plant dyeing technology and polyphenol processing, maintaining color fastness while maintaining color development or functionality is an essential condition for commercialization and widespread use. Advances have been made in techniques to improve and develop functions.
しかし、草木染めは、上水道発達以前より古くから行われ、上水道が発達した後へそのまま受け継がれている伝統技法であることから、染色布が塩素に晒されることを想定していない。また、近年発達したポリフェノール加工技術においても、商習慣の中で提示される最終納入先の要求対象に耐塩素性が含まれないことが一般的であり、プールで使用する水着等のような特殊な用途のものを除いては、耐塩素性についての技術検討を求められることは少ない。このようなことから、草木染め及びポリフェノール加工技術では、耐光、洗濯、汗、摩擦等の項目に関する堅牢度については検討されるが、塩素に対する耐久性については注目されず、塩素堅牢度の改良については十分に検討されていない。 However, plant dyeing is a traditional technique that has been carried out since before the development of the waterworks, and has been passed on since the development of the waterworks, so it is not assumed that the dyed fabric will be exposed to chlorine. Also, in polyphenol processing technology that has been developed in recent years, it is common that the requirements of the final delivery destination presented in business customs do not include chlorine resistance, and special features such as swimwear used in pools. Except for special applications, there is little demand for technical studies on chlorine resistance. For this reason, in plant dyeing and polyphenol processing technologies, fastness regarding items such as light resistance, washing, sweat, and friction are examined, but attention is not paid to durability against chlorine, and improvement of chlorine fastness. Has not been fully studied.
一方、一般的な化学染色による衣類用繊維染色品については、塩素堅牢度を向上させる既存の方法として、ジアミン類及び／又はタンニン酸で処理する方法（例えば、下記特許文献１）、ポリカチオン物質（ε−ポリリジン）を用いる方法（例えば、下記特許文献２）、樹脂類とチオ尿素誘導体で処理する方法（例えば、下記特許文献３）、樹脂類と尿素、グアニジン系化合物で処理する方法（例えば、下記特許文献４）、アリルアミン系ポリマーで処理する方法（例えば、下記特許文献5）、ポリエチレンポリアミンとエピハロヒドリンを縮合させたポリマーで処理する方法（例えば、下記特許文献6）、エピハロヒドリン−ヒドラジド系化合物の縮合物を用いる方法（例えば、下記特許文献7）等が提案されている。又、塩素堅牢度を向上させるためのフィックス剤として、綿反応染色のフィックス剤や、合成タンニン系、天然タンニン系のフィックス剤が市販されている。 On the other hand, with regard to textile dyeing for clothing by general chemical dyeing, as an existing method for improving chlorine fastness, a method of treating with diamines and / or tannic acid (for example, Patent Document 1 below), polycationic substance A method using (ε-polylysine) (for example, the following Patent Document 2), a method for treating with a resin and a thiourea derivative (for example, the following Patent Document 3), a method for treating with a resin and urea or a guanidine compound (for example, , The following patent document 4), a method of treating with an allylamine polymer (for example, the following patent document 5), a method of treating with a polymer obtained by condensing a polyethylene polyamine and an epihalohydrin (for example, the following patent document 6), an epihalohydrin-hydrazide compound. A method using a condensate of (for example, Patent Document 7 below) has been proposed. Further, as a fixing agent for improving chlorine fastness, a cotton reactive dyeing fixing agent, a synthetic tannin-based natural tannin-based fixing agent, and the like are commercially available.
現代の消費生活においては、家庭での洗濯は一般に水道水で行われるので、繊維製品が塩素に晒される機会は多い。従って、繊維製品について広く耐塩素性を持たせる必要があり、草木染めやポリフェノール加工技術においても、特殊用途のものに限らず、幅広く塩素堅牢度の改善を進めることは重要である。 In modern consumer life, washing at home is generally done with tap water, so textiles are often exposed to chlorine. Therefore, it is necessary to make the textiles widely resistant to chlorine, and it is important to improve the chlorine fastness in a wide range not only for special purposes, but also in plant dyeing and polyphenol processing techniques.
草木染めやポリフェノール加工繊維の塩素耐性を改善するために、前述した一般的な化学染色繊維衣類製品用の塩素堅牢度向上用フィックス剤を使用すると、塩素耐性の向上と引き換えに、耐光性の劣化や色相の変化を引き起こしたり、ポリフェノールが生地から脱離する等の問題が生じる。また、合成タンニン系、天然タンニン系のフィックス剤の場合は、フィックス剤自体が濃褐色であるために加工変色が問題になり、使用に際しては色目の制限を受け易い。 In order to improve the chlorine resistance of plant-dyed and polyphenol-processed fibers, using the above-mentioned fix agent for improving the fastness of chlorine for chemically dyed textile clothing products, the light resistance deteriorates in exchange for the improvement of chlorine resistance. Or a change in hue, or a problem such as polyphenol detachment from the fabric occurs. Further, in the case of a synthetic tannin-based or natural tannin-based fixing agent, the fixing agent itself is dark brown, so processing discoloration becomes a problem, and it is easy to be restricted in color when used.
従って、上述のような問題を生じることなく、草木染めやポリフェノール加工繊維の塩素堅牢度を改善可能な処理方法を見出す必要がある。 Therefore, there is a need to find a treatment method that can improve the chlorine fastness of vegetation dyeing and polyphenol processed fibers without causing the above-mentioned problems.
本発明の課題は、繊維にポリフェノールを加工するに際し、発色性、機能性、安全性、耐光性、耐洗濯性を維持しつつ耐塩素性を改善し、現代の消費生活に適合した堅牢性を備えるポリフェノール加工繊維を提供することである。 The object of the present invention is to improve the chlorine resistance while maintaining the color development, functionality, safety, light resistance and washing resistance when processing polyphenols into fibers, and to achieve robustness adapted to the modern consumer life. It is to provide a polyphenol processed fiber provided.
上記課題を解決するために、染着繊維の処理に使用される様々な処理剤成分について検討を重ねたところ、加工助剤として用いられる成分を利用してポリフェノール加工繊維の塩素堅牢度を改善することが可能な状況を見出し、本発明のポリフェノール加工繊維の製造方法に至った。 In order to solve the above-mentioned problems, various treatment agent components used in the treatment of dyed fibers have been studied, and the chlorine fastness of polyphenol processed fibers is improved by utilizing components used as processing aids. The present inventors have found a possible situation, and have reached the method for producing a polyphenol processed fiber of the present invention.
本発明の一態様によれば、ポリフェノール加工繊維の製造方法は、ポリフェノールに接触した繊維を、フェニルアミド化合物のアニオン性水性分散液で処理することを要旨とする。 According to one aspect of the present invention, a method for producing a polyphenol processed fiber is characterized in that a fiber in contact with polyphenol is treated with an anionic aqueous dispersion of a phenylamide compound.
本発明によれば、ポリフェノール加工繊維の発色性、機能性、安全性、耐光性、耐洗濯性を維持しつつ耐塩素性を改善することができるので、ポリフェノールの機能性を活かしつつ塩素堅牢度の向上したポリフェノール加工繊維を提供できる。従って、ポリフェノールの機能性を利用した製品の用途開発に有用であり、衣類一般に限ることなく、繊維を利用した様々な製品に、抗菌性、消臭性、抗酸化性などのポリフェノールの機能を付与して高品質の製品を提供することが可能となる。 According to the present invention, it is possible to improve the chlorine resistance while maintaining the color developability, functionality, safety, light resistance, and washing resistance of the polyphenol-processed fiber. Improved polyphenol processed fiber can be provided. Therefore, it is useful for application development of products that utilize the functionality of polyphenols, and not only for clothing in general, but also for the addition of polyphenol functions such as antibacterial, deodorant, and antioxidant properties to various products that use fibers. It becomes possible to provide high quality products.
染色繊維の塩素による変退色は、活性塩素による酸化退色によるものであり、特に木綿は、繊維が活性塩素を吸着し易い性質を有するために他の繊維より問題が生じ易い。 The discoloration of the dyed fiber due to chlorine is due to the oxidative discoloration due to active chlorine, and in particular, cotton is more prone to problems than other fibers because the fiber has the property of easily adsorbing active chlorine.
ポリフェノールは、抗酸化物質として知られているが、換言すれば、酸化物質と反応し易く、従って、活性塩素による酸化退色を受け易い。実際、草木染め品や従来のポリフェノール加工繊維について塩素堅牢度の測定（JIS L0884、塩素処理水堅牢度試験Ａ法）を行うと、１級から２級程度の極めて低い等級判定となり、草木染めやポリフェノール加工繊維のポリフェノールは耐塩素性が低いことが明らかである。 Polyphenols are known as antioxidants. In other words, polyphenols easily react with oxidizing substances, and are therefore susceptible to oxidative fading due to active chlorine. In fact, when we measure the chlorine fastness (JIS L0884, chlorinated water fastness test A method) for plant-dyed products and conventional polyphenol-processed fibers, we get an extremely low grade rating of grade 1 to 2, It is clear that the polyphenol of the polyphenol processed fiber has low chlorine resistance.
ポリフェノール加工繊維に従来の塩素堅牢度向上用フィックス剤を使用すると、色相の変化が生じることがあり、これはｐＨ変化に起因する作用である。又、ポリフェノールが生地から脱離することもあり、これは、カチオン物質との作用によるものであり、カチオン物質とポリフェノールとが結合して凝集物を生成して生地を汚染する場合もある。何れもフェノール性水酸基の性質に関連するので、ポリフェノール加工繊維の耐塩素性を改善する際には、フェノール性水酸基の特性を十分に考慮する必要がある。 When a conventional fixing agent for improving the fastness of chlorine is used for a polyphenol processed fiber, a hue change may occur, which is an effect caused by a pH change. In addition, polyphenol may be detached from the dough, which is due to the action of the cationic substance, and the cationic substance and polyphenol may combine to form an aggregate to contaminate the dough. Since both are related to the properties of the phenolic hydroxyl group, it is necessary to fully consider the characteristics of the phenolic hydroxyl group when improving the chlorine resistance of the polyphenol processed fiber.
本発明では、上記を鑑みて検討を重ねた結果、特定状態のフェニルアミド化合物がポリフェノール加工繊維の塩素堅牢度の改善に有用であることが判明し、ポリフェノールを接触させた繊維に、上記フェニルアミド化合物を用いた処理を施すことによって、発色性、機能性、安全性、耐光性、耐洗濯性を維持しつつ耐塩素性が向上したポリフェノール加工繊維を提供可能であることを見出した。 In the present invention, as a result of repeated studies in view of the above, it has been found that a phenylamide compound in a specific state is useful for improving the chlorine fastness of a polyphenol-processed fiber. It has been found that by applying a treatment using a compound, it is possible to provide a polyphenol-processed fiber having improved chlorine resistance while maintaining color development, functionality, safety, light resistance and washing resistance.
以下に、本発明のポリフェノール加工繊維の製造方法について説明する。尚、以下の記載において、ポリフェノール加工繊維は、一般的な草木染め品等を含む、繊維上にポリフェノールを有する繊維を広く包含するものとし、染色又はポリフェノール加工の種類や、天然繊維又は化学繊維の区別を問わない。具体的には、使用可能なポリフェノールとして、一般的に草木染めやポリフェノール加工に用いられる、茶、柿、ざくろの他、ブドウ、グアバ、ローズヒップ、そば、小豆、オリーブ、リンゴ、シソ、ビワ葉、柿、クリ、コーヒー、シナモン、ベリー類などの各種植物の葉、果実、種子、花、茎、根等から抽出されるポリフェノールが挙げられ、このようなものから適宜選択することができる。茶ポリフェノールは、生葉、加工茶（不発酵茶、半発酵茶、発酵茶）、抽出エキス、抽出物パウダー、抽出後残渣などに含まれるものを利用することができ、形態は問わない。茶ポリフェノール及びブドウポリフェノールは、その機能性において特に優れており、好ましい。又、使用可能な繊維の種類についても、セルロース繊維、動物性繊維、ポリエステル繊維、アセテート繊維、ナイロン繊維、アクリル繊維、レーヨン繊維、ポリプロピレン繊維、ポリ塩化ビニル繊維、ポリ乳酸繊維、ポリウレタン繊維等の各種繊維が挙げられ、これらから適宜選択して本発明を適用することができる。 Below, the manufacturing method of the polyphenol processed fiber of this invention is demonstrated. In the following description, polyphenol-processed fibers widely include fibers having polyphenol on the fibers, including general plant-dyed products, etc., and the types of dyeing or polyphenol processing, natural fibers or chemical fibers It doesn't matter. Specifically, as polyphenols that can be used, it is commonly used for plant dyeing and polyphenol processing, as well as tea, grapes, pomegranates, grapes, guava, rose hips, buckwheat, red beans, olives, apples, perilla, loquat leaves. , Polyphenols extracted from leaves, fruits, seeds, flowers, stems, roots, and the like of various plants such as strawberries, chestnuts, coffee, cinnamon, berries, etc., can be selected as appropriate. As tea polyphenol, those contained in fresh leaves, processed tea (non-fermented tea, semi-fermented tea, fermented tea), extract extract, extract powder, post-extraction residue, etc. can be used, and the form is not limited. Tea polyphenols and grape polyphenols are particularly excellent in their functionality and are preferred. Also, the types of fibers that can be used are cellulose fibers, animal fibers, polyester fibers, acetate fibers, nylon fibers, acrylic fibers, rayon fibers, polypropylene fibers, polyvinyl chloride fibers, polylactic acid fibers, polyurethane fibers, etc. Examples thereof include fibers, and the present invention can be applied by appropriately selecting them.
繊維に接触させたポリフェノールは、繊維表面に極性基があると、ポリフェノールの水酸基との間に水素結合やイオン結合を介した配位、相互作用等を生じ、繊維上のポリフェノールの定着・安定化を補う作用をすると考えられる。ポリフェノール加工繊維の塩素堅牢度を改善するには、このような結合を破壊することなくポリフェノールを保護する必要がある。 If the polyphenol contacted with the fiber has a polar group on the fiber surface, it will coordinate and interact with the hydroxyl group of the polyphenol via a hydrogen bond or ionic bond, thereby fixing and stabilizing the polyphenol on the fiber. It is thought to act to supplement In order to improve the chlorine fastness of the polyphenol-processed fiber, it is necessary to protect the polyphenol without breaking such bonds.
本発明においては、塩素堅牢度を改善（堅牢化）するための処理剤として、エステル基を有するフェニルアミド化合物の水性分散液で、フェニルアミド化合物の分子内又は分子外に共存して分散する弱酸性アニオンを含有するものを使用する。本発明で使用する堅牢化処理剤が塩素堅牢度を改善するメカニズムは、以下のようなことが考えられる。 In the present invention, as a treating agent for improving (fastening) chlorine fastness, an aqueous dispersion of a phenylamide compound having an ester group is a weak dispersion that coexists in and out of the molecule of the phenylamide compound. Those containing acidic anions are used. The mechanism by which the fastening treatment agent used in the present invention improves the chlorine fastness is considered as follows.
ポリフェノールの抗酸化作用の反応メカニズムは完全には解明されてはいないが、メカニズムの一部として、フェノール性水酸基の水素原子移動に基づく反応と、電子移動に基づく反応とがある。水素原子移動による反応は、水酸基から供給される水素原子ラジカルと活性塩素ラジカルが反応して失活するもので、非プロトン性媒体中で進行するのに対し、電子移動による反応は、水酸基から供給される電子を活性塩素ラジカルが受容して塩素イオンとなって失活するもので、プロトン性媒体中で進行し、金属イオンによって反応が促進される。草木染めやポリフェノール加工が施される水系において、アニオンの供給は、フェノール性水酸基の電離抑制を可能とするので、フェノール性水酸基の電子移動を抑制することによってポリフェノールの塩素堅牢度の改善に寄与すると考えられる。この際、使用するアニオンがカルボン酸基、リン酸基等の弱酸性アニオンであると、ｐＨ変化によるポリフェノールの呈色性の変化が抑制される。また、媒体に溶解するアニオンの場合は、繊維に浸透してポリフェノールの染着自体に影響を与え得るが、この点は、分散性のアニオンを用いることによって解消し、繊維上のポリフェノールの周囲から穏やかに作用する。 Although the reaction mechanism of the antioxidant action of polyphenols has not been completely elucidated, there are reactions based on hydrogen atom transfer of phenolic hydroxyl groups and reactions based on electron transfer as part of the mechanism. In the reaction by hydrogen atom transfer, the hydrogen atom radical supplied from the hydroxyl group reacts with the active chlorine radical and deactivates, and proceeds in an aprotic medium, whereas the reaction by electron transfer is supplied from the hydroxyl group. The active chlorine radical accepts the generated electrons and deactivates them as chlorine ions, which proceeds in a protic medium, and the reaction is promoted by metal ions. In an aqueous system where plant dyeing or polyphenol processing is applied, the supply of anions makes it possible to suppress the ionization of phenolic hydroxyl groups, and thus contributes to improving the chlorine fastness of polyphenols by suppressing the electron transfer of phenolic hydroxyl groups. Conceivable. At this time, when the anion to be used is a weakly acidic anion such as a carboxylic acid group or a phosphoric acid group, a change in the colorability of the polyphenol due to a change in pH is suppressed. In the case of an anion dissolved in the medium, it can penetrate into the fiber and affect the dyeing of the polyphenol itself, but this point can be solved by using a dispersible anion, and from the periphery of the polyphenol on the fiber. Acts gently.
フェニルアミド化合物は、フェニル基の疎水性及びアミド基の難溶性と、堅固なフェニルアミド骨格とにより、水溶性が低く凝固性を呈し易い分子構造であるが、エステル基を有すると、柔軟性及び極性が加わって液状化し易くなり、水性乳濁液を構成し易くなる。フェニル基はポリフェノールとの親和性を有し、ポリフェノールに近接して疎水性の障壁となって塩素の接触を阻害することによってポリフェノールを物理的に保護すると考えられる。従って、弱酸性アニオンが、フェニルアミド化合物の分子内又は分子外に共存して分散することによって、フェノール性水酸基の電離抑制とポリフェノールの疎水保護とに効果的に作用する。 The phenylamide compound has a molecular structure with low water solubility and easy coagulation due to the hydrophobicity of the phenyl group and the poor solubility of the amide group and the firm phenylamide skeleton. Polarity is added and it becomes easy to liquefy, and it becomes easy to constitute an aqueous emulsion. The phenyl group has an affinity for polyphenols and is considered to physically protect the polyphenols by blocking the contact of chlorine with a hydrophobic barrier adjacent to the polyphenols. Accordingly, the weakly acidic anion coexists in and out of the molecule of the phenylamide compound, thereby effectively acting to suppress ionization of the phenolic hydroxyl group and to protect the hydrophobicity of the polyphenol.
上記に従って、フェニルアミド化合物は、具体的には、フェニルアミド骨格を有し、アミド基の窒素原子及びカルボニル炭素原子に各々結合する置換基を有し、これらの置換基は、各々、炭素数が１〜５０の鎖状又は環状の飽和脂肪族基であって、酸素原子及び／又は窒素原子を含有しても良く、芳香族基が結合しても良い。少なくとも１つの置換基にはエステル基が含まれ、エステル基は鎖状であっても環状基を構成しても良い。上記置換基がエーテル結合を有すると分子の柔軟性が向上するので好ましい。フェニルアミド骨格のフェニル基は、１個以上のメチル基又はハロゲン原子で置換されていても良く、分子の嵩高さによって活性塩素の排除効果が高まる。フェニルアミド化合物の具体例としては、メタラキシル［メチル N-(2-メトキシアセチル)-N-(2,6-キシリル)-DL-アラニネート］、オキサジキシル［2-メトキシ-N-(2-オキソ-1,3-オキサゾリジン-3-イル)アセト-2',6'-キシリジド］、オフレース［(±)-α-2-クロロ-N-(2,6-キシリルアセトアミド)-γ-ブチロラクトン］、ベナラキシル［メチル N-フェニルアセチル-N-(2,6-キシリル)-DL-アラニネート］、フララキシル［メチル N-(2-フロイル)-N-(2,6-キシリル)-DL-アラニネート］、シプロフラン［(±)-α-{N-(3-クロロフェニル)シクロプロパンカルボキサミド}-γ-ブチロラクトン］等が挙げられ、これらは抗菌剤成分としても使用可能な化合物である。 In accordance with the above, the phenylamide compound specifically has a phenylamide skeleton, and has substituents bonded to the nitrogen atom and the carbonyl carbon atom of the amide group, respectively, each of these substituents having a carbon number. 1 to 50 chain or cyclic saturated aliphatic groups, which may contain an oxygen atom and / or a nitrogen atom, and may be bonded to an aromatic group. The at least one substituent includes an ester group, and the ester group may be a chain or may form a cyclic group. It is preferable that the substituent has an ether bond because the flexibility of the molecule is improved. The phenyl group of the phenylamide skeleton may be substituted with one or more methyl groups or halogen atoms, and the effect of eliminating active chlorine is enhanced by the bulk of the molecule. Specific examples of phenylamide compounds include metalaxyl [methyl N- (2-methoxyacetyl) -N- (2,6-xylyl) -DL-alaninate], oxadixyl [2-methoxy-N- (2-oxo-1 , 3-Oxazolidin-3-yl) aceto-2 ′, 6′-xylidide], off-race [(±) -α-2-chloro-N- (2,6-xylylacetamido) -γ-butyrolactone], Benalaxyl [methyl N-phenylacetyl-N- (2,6-xylyl) -DL-alaninate], furaraxyl [methyl N- (2-furoyl) -N- (2,6-xylyl) -DL-alaninate], cyprofuran [(±) -α- {N- (3-chlorophenyl) cyclopropanecarboxamide} -γ-butyrolactone] and the like, which are compounds that can also be used as an antibacterial agent component.
本発明において使用する堅牢化処理剤は、上記フェニルアミド化合物及びアニオンの作用を阻害しない限りにおいて、更に水分散性の高分子成分を含んでも良く、カルボキシ基やリン酸基などを含有するアニオン系高分子等は、アニオンを供給するキャリアとして作用する。また、ポリフェノールの物理的保護体としても作用する。このような点から好ましい高分子成分として、カルボキシ基を分子内又は分子外に含有するアクリル系重合体又は共重合体等の高分子が挙げられる。従って、本発明における堅牢化処理剤として、例えば、アニオン型アクリル樹脂エマルジョン液に上記フェニルアミド化合物を配合したものなどのような、アニオン性高分子分散液をベースとしたフェニルアミド化合物含有水性分散液を好適に利用できる。このような形態の高分子分散液では、アニオン及びフェニルアミド化合物は、水中に溶解せずに分散高分子と共に存在するので、繊維内部にまでは浸透し難く、繊維表面のポリフェノールの外周から接触・作用する。そのため、繊維内部からポリフェノールの染着座席を奪ってポリフェノールを離脱させるようなことを避けることができ、又、分散粒子から穏やかに作用し、ポリフェノールに急激な変化を及ぼさない。分散安定性等の点から、堅牢化処理剤は、不揮発分濃度が１〜５０質量％程度、好ましくは５〜３０質量％であると好適であり、ポリフェノールに対する作用の点から、処理剤のｐＨが１．０〜７．０程度、好ましくは２．５〜５．５程度であると好適である。不揮発分には、フェニルアミド化合物、アニオン成分（フェニルアミド化合物から分離して存在する場合）や、上述の高分子成分が含まれる。 The fastening treatment agent used in the present invention may further contain a water-dispersible polymer component as long as the action of the phenylamide compound and the anion is not inhibited, and an anionic system containing a carboxy group or a phosphate group. The polymer or the like acts as a carrier for supplying an anion. It also acts as a physical protector for polyphenols. From such a point, preferred polymer components include polymers such as acrylic polymers or copolymers containing a carboxy group in the molecule or outside the molecule. Accordingly, as the fastening treatment agent in the present invention, for example, an aqueous dispersion containing a phenylamide compound based on an anionic polymer dispersion such as an anionic acrylic resin emulsion mixed with the phenylamide compound. Can be suitably used. In such a polymer dispersion, the anion and the phenylamide compound do not dissolve in water and exist together with the dispersed polymer, so that they do not easily penetrate into the inside of the fiber, and contact / Works. Therefore, it is possible to avoid taking the polyphenol dyeing seat from the inside of the fiber and detaching the polyphenol, and it acts gently from the dispersed particles and does not cause a rapid change in the polyphenol. From the viewpoint of dispersion stability and the like, the fastening treatment agent preferably has a non-volatile content concentration of about 1 to 50% by mass, preferably 5 to 30% by mass. Is about 1.0 to 7.0, preferably about 2.5 to 5.5. The nonvolatile component includes a phenylamide compound, an anion component (when present separately from the phenylamide compound), and the above-described polymer component.
上述のような堅牢化処理剤を、ポリフェノールにより染着又は加工された繊維に接触させることにより、繊維上のポリフェノールの塩素堅牢度が向上する。処理剤による堅牢化は、ポリフェノールが繊維に接触した後であればよく、ポリフェノールによる染着又は加工後に余分なポリフェノールを除去して個別に施しても、或いは、染着又は加工に連続してポリフェノールが共存する状態で行っても良い。つまり、ポリフェノールを繊維に染着した浴中に上記処理剤を添加して行っても良い。堅牢化処理は、ｐＨ４．１〜７．０の弱酸性〜中性で行うことが望ましい。 By bringing the fastening treatment agent as described above into contact with a fiber dyed or processed with polyphenol, the chlorine fastness of the polyphenol on the fiber is improved. Fastening with the treatment agent may be performed after the polyphenol comes into contact with the fiber. After the polyphenol is dyed or processed, the polyphenol may be applied individually after removing the extra polyphenol, or continuously after the dyeing or processing. May be performed in a state where coexists. That is, the treatment agent may be added to a bath in which polyphenols are dyed on fibers. It is desirable that the fastening treatment is performed at a slightly acidic to neutral pH of 4.1 to 7.0.
ポリフェノール加工繊維は、繊維をポリフェノール水溶液に接触させてポリフェノールを染着し、余分のポリフェノールを水洗除去することによって得られるが、綿、ポリエステルなどのポリフェノールが脱離し易い繊維の場合は、予め、カチオン剤、及び、必要に応じてアルカリを繊維に接触させて繊維表面を活性化し、十分に水洗した後にポリフェノール加工を施す。綿のポリフェノール加工は、例えば、以下のように実施される。 Polyphenol processed fiber is obtained by bringing the fiber into contact with an aqueous solution of polyphenol, dyeing the polyphenol, and washing away the excess polyphenol with water. The surface of the fiber is activated by bringing the agent and, if necessary, an alkali into contact with the fiber, and after sufficiently washing with water, polyphenol processing is applied. The polyphenol processing of cotton is implemented as follows, for example.
詳細には、精錬・漂白等を経た繊維生地を水に浸し、カチオン剤水溶液を繊維に対して１０質量％程度の割合で添加して１０分程度繊維に接触させ、水酸化ナトリウム等のアルカリを繊維に対して２質量％程度の割合で加えて含浸した後、８０℃程度まで徐々に昇温して３０分程度維持する。この後、十分に水洗を行って、繊維を再度水に浸し、繊維に対してポリフェノールが０．１〜７質量％程度、好ましくは０．３〜２質量％、より好ましくは０．５質量％程度となる割合でポリフェノール水溶液を添加し、３０℃程度に加熱してｐＨ６〜７で２０分程度ポリフェノールを繊維に染着し、水洗して余分のポリフェノールを除去する。 Specifically, the fiber fabric that has undergone refining and bleaching is soaked in water, and an aqueous cationic agent solution is added at a ratio of about 10% by mass with respect to the fiber and brought into contact with the fiber for about 10 minutes. After adding and impregnating at a ratio of about 2% by mass with respect to the fiber, the temperature is gradually raised to about 80 ° C. and maintained for about 30 minutes. After this, it is washed thoroughly with water, and the fiber is again immersed in water. The polyphenol is about 0.1 to 7% by mass, preferably 0.3 to 2% by mass, more preferably 0.5% by mass, based on the fiber. A polyphenol aqueous solution is added at a ratio of approximately, heated to about 30 ° C., dyed on the fiber for about 20 minutes at pH 6-7, washed with water to remove excess polyphenol.
ポリフェノール加工された繊維の後加工として上記処理剤による堅牢化を行う場合、水に浸した繊維に堅牢化処理剤を添加して、ｐＨ４．５以上の弱酸性域（ｐＨ７未満）、好ましくはｐＨ６〜６．９）でポリフェノール加工繊維を接触させ、３５〜９５℃程度、好ましくは５０〜８０℃程度、より好ましくは６０℃前後に加熱することによって好適に堅牢化処理が施される。堅牢化処理剤の添加量は、繊維に対して０．１〜１０質量％程度、好ましくは０．５〜７質量％程度、さらに好ましくは１〜３質量％程度となるように設定し、処理時間は概して１０〜６０分程度、好ましくは３０分前後であり、処理後の繊維は十分に水洗する。 When fastening with the above-mentioned treatment agent as post-processing of the polyphenol-processed fiber, the fastening treatment agent is added to the fiber soaked in water, and the pH is 4.5 or more weakly acidic region (less than pH 7), preferably pH 6 To 6.9), the polyphenol-processed fibers are brought into contact with each other and heated to about 35 to 95 ° C., preferably about 50 to 80 ° C., more preferably about 60 ° C., whereby the fastening treatment is suitably performed. The addition amount of the fastening treatment agent is set to be about 0.1 to 10% by mass, preferably about 0.5 to 7% by mass, and more preferably about 1 to 3% by mass with respect to the fiber. The time is generally about 10 to 60 minutes, preferably around 30 minutes, and the treated fibers are thoroughly washed with water.
綿等のポリフェノールが脱離し易い繊維に対して、ポリフェノール加工と連続して同浴中で上記処理剤による堅牢化を行う場合は、ｐＨ３〜１１の範囲において処理が可能であり、ポリフェノールの性質を考慮するとｐＨ４．１以上の弱酸性域（ｐＨ７未満）が好ましい。同浴での処理では、繊維に対するポリフェノールの親和性を高めて定着し易くするために媒染剤を使用すると好ましい。例えば、以下のように金属媒染剤として錫酸ナトリウムを用いて実施することができる。 For fibers such as cotton, from which polyphenols are easily detached, when the above treatment agent is fastened continuously in the same bath as polyphenol processing, the treatment can be performed in the range of pH 3 to 11, and the properties of polyphenols can be reduced. In consideration, a weakly acidic range of pH 4.1 or higher (less than pH 7) is preferable. In the treatment in the same bath, it is preferable to use a mordant in order to increase the affinity of the polyphenol with respect to the fibers to facilitate fixing. For example, it can be carried out using sodium stannate as a metal mordant as follows.
詳細には、精錬・漂白等を経た繊維生地を水に浸し、ポリフェノール水溶液を、繊維に対してポリフェノールが０．１〜７質量％程度、好ましくは０．５〜３．０質量％程度となる割合で添加して最初にポリフェノールを繊維に接触させる。この後、加熱して３５〜９５℃程度、好ましくは８０〜９５℃程度まで昇温し、クエン酸及び錫酸ナトリウムを溶解した水溶液を、繊維に対してクエン酸１〜１０質量％程度、好ましくは２〜４質量％程度、錫酸ナトリウム０．５〜５質量％程度、好ましくは１〜２質量％程度となる割合で添加して１０分程度維持することによってポリフェノールを染着する。この後、堅牢化処理剤を添加して、ｐＨ３〜１１程度、好ましくはｐＨ４〜５程度で温度を３５〜９５℃程度、好ましくは８０〜９５℃程度に維持して処理剤を３０分程度繊維に接触させると好適に処理できる。処理を経た繊維は適宜水洗する。堅牢化処理剤の添加量は、繊維に対して０．２〜７質量％程度、好ましくは０．５〜３質量％程度となるように設定するとよい。 In detail, the fiber dough which passed through refining, bleaching, etc. is immersed in water, and polyphenol aqueous solution becomes about 0.1-7 mass% with respect to fiber, Preferably it is about 0.5-3.0 mass%. The polyphenol is first contacted with the fiber by adding in proportions. Thereafter, the mixture is heated to a temperature of about 35 to 95 ° C., preferably about 80 to 95 ° C., and an aqueous solution in which citric acid and sodium stannate are dissolved is about 1 to 10% by mass of citric acid, preferably about Is added at a ratio of about 2 to 4% by mass, sodium stannate about 0.5 to 5% by mass, preferably about 1 to 2% by mass and maintained for about 10 minutes to dye polyphenols. Thereafter, the fastening treatment agent is added, and the fiber is kept for about 30 minutes while maintaining the temperature at about 35 to 95 ° C., preferably about 80 to 95 ° C. at about pH 3 to 11, preferably about 4 to 5. It can process suitably when it is made to contact. The treated fiber is washed with water as appropriate. The addition amount of the fastening treatment agent may be set to about 0.2 to 7% by mass, preferably about 0.5 to 3% by mass with respect to the fiber.
上述において、ポリフェノールは、一般的に草木染めやポリフェノール加工等で用いられる各種ポリフェノールから適宜選択して利用すればよい。カテキン等の茶由来ポリフェノールやブドウ由来のポリフェノールは、その機能性の点で特に優れており、好ましい。 In the above description, the polyphenol may be appropriately selected from various polyphenols generally used in plant dyeing or polyphenol processing. Tea-derived polyphenols such as catechins and grape-derived polyphenols are particularly excellent in terms of their functionality and are preferred.
上述の堅牢化処理を施したポリフェノール加工繊維は、塩素堅牢度が３級程度に改善さる。又、河合式パッチテストで準陰性を示し、エコテックス溶出試験でも重金属・農薬成分は検出限界以下であるので安全性も高い。ポリフェノールの機能である抗菌性、消臭性、抗酸化性についても良好に発揮し、ＵＶカット効果も好適である。 The polyphenol processed fiber subjected to the above-mentioned fastening treatment has improved chlorine fastness to about the third grade. In addition, the Kawai-type patch test shows semi-negative, and even in the Oeko-Tex dissolution test, heavy metals and pesticide components are below the detection limit, so safety is high. The anti-bacterial properties, deodorizing properties, and antioxidant properties that are functions of polyphenols are also exhibited well, and the UV cut effect is also suitable.
以下の作業に従って、ポリフェノール加工繊維（試料１〜５）、フェニルアミドによる堅牢化処理を施したポリフェノール加工繊維（試料１Ａ、２Ａ〜２Ｃ、３Ａ〜６Ａ）及び市販のフィックス剤処理を施したポリフェノール加工繊維（試料７〜９）を作成し、塩素堅牢度及びポリフェノールの色変化の有無を調べた。 In accordance with the following operations, polyphenol processed fibers (samples 1 to 5), polyphenol processed fibers subjected to fastening treatment with phenylamide (samples 1A, 2A to 2C, 3A to 6A), and polyphenol processing subjected to a commercially available fix agent treatment Fibers (Samples 7 to 9) were prepared, and examined for the fastness of chlorine and the presence or absence of color change of the polyphenol.
（試料１）
精錬漂白を行った綿生地１kgを、染浴中で約１５Ｌの水に浸し、十分に水を含浸させた。これに、カチオン剤（商品名：カチオノンＫＣＮ、一方社油脂工業社製４級アンモニウム塩）１００ｇを加えて１０分間攪拌した。更に、約１Ｌの水に水酸化ナトリウム２０ｇを溶解した溶液を調製して染浴に加え、１０分間攪拌した。約３Ｌの水を追加して染浴中の液量を２０Ｌに調整し、加熱して８０℃まで昇温し、温度を維持して３０分間攪拌しながら綿生地を十分に浸漬した。この後、染浴の液を排出し、流水で綿生地を念入りに水洗して中和しながら、洗浄水を排出した。
(Sample 1)
1 kg of cotton fabric subjected to refining and bleaching was immersed in about 15 L of water in a dyeing bath and sufficiently impregnated with water. To this was added 100 g of a cation agent (trade name: Cationone KCN, quaternary ammonium salt manufactured by Yushi Kogyo Co., Ltd.) and stirred for 10 minutes. Further, a solution in which 20 g of sodium hydroxide was dissolved in about 1 L of water was prepared, added to the dye bath, and stirred for 10 minutes. About 3 L of water was added to adjust the amount of liquid in the dye bath to 20 L, heated to 80 ° C., and the cotton fabric was sufficiently immersed while stirring for 30 minutes while maintaining the temperature. Thereafter, the dyebath solution was discharged, and the washing water was discharged while the cotton fabric was carefully washed with running water and neutralized.
染浴に約１５Ｌの水を投入して綿生地を浸した。茶抽出ポリフェノール（商品名：テアフラン３０Ｆ、株式会社伊藤園製）５ｇを約１Ｌの水に溶解して染浴に投入し、水を追加して染浴の液量を２０Ｌに調整した。これを加熱して３０℃まで昇温し、温度を維持して３０分間攪拌しながら綿生地を十分に浸漬した。この後、染浴の液を排出して、流水で綿生地を念入りに水洗し、綿生地を取り出して脱水、乾燥することにより、ポリフェノール加工綿布を得た。 About 15 L of water was poured into the dye bath to immerse the cotton fabric. 5 g of tea-extracted polyphenol (trade name: Teafuran 30F, manufactured by ITO EN Co., Ltd.) was dissolved in about 1 L of water and added to the dye bath, and water was added to adjust the amount of the dye bath to 20 L. This was heated and heated up to 30 ° C., and the cotton fabric was sufficiently immersed while maintaining the temperature and stirring for 30 minutes. Thereafter, the dyebath solution was discharged, the cotton fabric was carefully washed with running water, the cotton fabric was taken out, dehydrated and dried to obtain a polyphenol-treated cotton fabric.
上述で得たポリフェノール加工綿布について、耐光堅牢度（JIS L0842）及び塩素堅牢度（JIS L0884 A法）を測定したところ、耐光堅牢度は３級、塩素堅牢度は１−２級であった。 When the light fastness (JIS L0842) and the chlorine fastness (JIS L0884 A method) of the polyphenol-treated cotton fabric obtained above were measured, the light fastness was grade 3 and the chlorine fastness was grade 1-2.
（試料１Ａ）
試料１で得たポリフェノール加工綿布１kgを、染浴中で約１５Ｌの水に浸し、十分に水を含浸させた。これに、分散性フェニルアミド処理剤（商品名：ＩＴＮ００３Ｍ、（株）竹内商店製アニオン性フェニルアミド系繊維加工剤、樹脂含有酸性水性液）２０ｇを添加して１０分間攪拌し、約４Ｌの水を追加して染浴の液量を２０Ｌに調整した（ｐＨ６．７）。これを加熱して５０℃まで昇温し、温度を維持して３０分間攪拌しながら綿生地を十分に浸漬した。この後、染浴の液を排出して、流水で綿生地を念入りに水洗し、綿生地を取り出して脱水、乾燥することにより、フェニルアミド処理後のポリフェノール加工綿布を得た。
(Sample 1A)
1 kg of the polyphenol-treated cotton fabric obtained in Sample 1 was immersed in about 15 L of water in a dye bath and sufficiently impregnated with water. To this, 20 g of a dispersible phenylamide treatment agent (trade name: ITN003M, an anionic phenylamide fiber processing agent manufactured by Takeuchi Shoten Co., Ltd., resin-containing acidic aqueous liquid) was added and stirred for 10 minutes, and about 4 L of water was added. Was added to adjust the amount of the dye bath to 20 L (pH 6.7). This was heated and heated up to 50 ° C., and the cotton fabric was sufficiently immersed while stirring for 30 minutes while maintaining the temperature. Thereafter, the dyebath solution was discharged, the cotton fabric was carefully washed with running water, the cotton fabric was taken out, dehydrated and dried to obtain a polyphenol-treated cotton fabric after phenylamide treatment.
得られたポリフェノール加工綿布について、耐光堅牢度及び塩素堅牢度を測定したところ、耐光堅牢度は３級、塩素堅牢度は３級であった。 When the light fastness and chlorine fastness of the obtained polyphenol-treated cotton fabric were measured, the light fastness was grade 3 and the chlorine fastness was grade 3.
（試料２）
精錬漂白を行った綿生地１kgを、染浴中で約１５Ｌの水に浸し、十分に水を含浸させた。これに、茶抽出ポリフェノール（商品名：テアフラン３０Ｆ、株式会社伊藤園製）５ｇを約１Ｌの水に溶解して投入し、これを加熱して８０℃まで昇温した。錫酸ナトリウム１０ｇ及びクエン酸２０ｇを約１Ｌの水に溶解した水溶液を染浴に投入し、水を追加して染浴の液量を２０Ｌに調整して、８０℃で３０分間攪拌しながら綿生地を十分に浸漬した。この後、染浴の液を排出して、流水で綿生地を念入りに水洗し、綿生地を取り出して脱水、乾燥することにより、ポリフェノール加工綿布を得た。
(Sample 2)
1 kg of cotton fabric subjected to refining and bleaching was immersed in about 15 L of water in a dyeing bath and sufficiently impregnated with water. To this, 5 g of tea-extracted polyphenol (trade name: Teafuran 30F, manufactured by ITO EN Co., Ltd.) was dissolved in about 1 L of water, and this was heated and heated to 80 ° C. An aqueous solution prepared by dissolving 10 g of sodium stannate and 20 g of citric acid in about 1 L of water is added to the dyeing bath, water is added to adjust the amount of the dyeing bath to 20 L, and cotton is stirred at 80 ° C. for 30 minutes. The dough was fully immersed. Thereafter, the dyebath solution was discharged, the cotton fabric was carefully washed with running water, the cotton fabric was taken out, dehydrated and dried to obtain a polyphenol-treated cotton fabric.
上述で得たポリフェノール加工綿布について、耐光堅牢度及び塩素堅牢度を測定したところ、耐光堅牢度は３級、塩素堅牢度は２−３級であった。 When the light fastness and chlorine fastness of the polyphenol-treated cotton fabric obtained above were measured, the light fastness was grade 3 and the chlorine fastness was grade 2-3.
（試料２Ａ）
精錬漂白を行った綿生地１kgを、染浴中で約１５Ｌの水に浸し、十分に水を含浸させた。これに、茶抽出ポリフェノール（商品名：テアフラン３０Ｆ、株式会社伊藤園製）５ｇを約１Ｌの水に溶解して投入し、これを加熱して８０℃まで昇温した。錫酸ナトリウム１０ｇ及びクエン酸２０ｇを約１Ｌの水に溶解した水溶液を染浴に投入し、水を追加して染浴の液量を２０Ｌに調整して、８０℃で１０分間攪拌しながら綿生地を十分に浸漬した。これに、分散性フェニルアミド処理剤（商品名：ＩＴＮ００３Ｍ、（株）竹内商店製アニオン性フェニルアミド系繊維加工剤、樹脂含有酸性水性液）３０ｇを添加して（ｐＨ４．５）、８０℃で３０分間攪拌した。この後、染浴の液を排出して、流水で綿生地を念入りに水洗し、綿生地を取り出して脱水、乾燥することにより、フェニルアミド処理したポリフェノール加工綿布を得た。
(Sample 2A)
1 kg of cotton fabric subjected to refining and bleaching was immersed in about 15 L of water in a dyeing bath and sufficiently impregnated with water. To this, 5 g of tea-extracted polyphenol (trade name: Teafuran 30F, manufactured by ITO EN Co., Ltd.) was dissolved in about 1 L of water, and this was heated and heated to 80 ° C. An aqueous solution obtained by dissolving 10 g of sodium stannate and 20 g of citric acid in about 1 L of water is added to the dyeing bath, water is added to adjust the amount of the dyeing bath to 20 L, and cotton is stirred at 80 ° C. for 10 minutes. The dough was fully immersed. To this was added 30 g of a dispersible phenylamide treating agent (trade name: ITN003M, an anionic phenylamide fiber processing agent, resin-containing acidic aqueous solution manufactured by Takeuchi Shoten Co., Ltd.) (pH 4.5) at 80 ° C. Stir for 30 minutes. Thereafter, the dye bath was discharged, the cotton fabric was carefully washed with running water, the cotton fabric was taken out, dehydrated and dried to obtain a phenylamide-treated polyphenol-treated cotton fabric.
得られたポリフェノール加工綿布について、耐光堅牢度及び塩素堅牢度を測定したところ、耐光堅牢度は３級、塩素堅牢度は３−４級であった。 When the light fastness and the chlorine fastness were measured for the obtained polyphenol-treated cotton fabric, the light fastness was grade 3 and the chlorine fastness was grade 3-4.
（試料２Ｂ）
試料２Ａの操作において、染浴に添加する分散性フェニルアミド処理剤の量を３０ｇから１００ｇに変更したこと以外は同様にして、フェニルアミド処理したポリフェノール加工綿布を作成した。尚、分散性フェニルアミド処理剤を添加した染浴において、液はｐＨ４．４であった。
(Sample 2B)
In the operation of Sample 2A, a phenylamide-treated polyphenol-treated cotton fabric was prepared in the same manner except that the amount of the dispersible phenylamide treatment agent added to the dye bath was changed from 30 g to 100 g. In the dye bath to which a dispersible phenylamide treating agent was added, the solution had a pH of 4.4.
得られたポリフェノール加工綿布について、塩素堅牢度を測定したところ、３−４級であった。但し、堅牢化処理中に、処理剤の過剰に起因すると思われる起泡によって処理液の溢れが生じ、作業の点で問題であった。 When the chlorine fastness of the obtained polyphenol-treated cotton fabric was measured, it was 3-4 grade. However, during the hardening process, the treatment liquid overflowed due to foaming that seems to be caused by excess of the treatment agent, which was a problem in terms of work.
（試料２Ｃ）
試料２Ａの操作において、染浴に添加する分散性フェニルアミド処理剤の量を３０ｇから１ｇに変更したこと以外は同様にして、フェニルアミド処理したポリフェノール加工綿布を作成した。尚、分酸性フェニルアミド処理剤を添加した染浴において、液はｐＨ５．１であった。
(Sample 2C)
In the operation of Sample 2A, a phenylamide-treated polyphenol-treated cotton fabric was prepared in the same manner except that the amount of the dispersible phenylamide treatment agent added to the dye bath was changed from 30 g to 1 g. In the dye bath to which the acidic phenylamide treating agent was added, the solution had a pH of 5.1.
得られたポリフェノール加工綿布について、塩素堅牢度を測定したところ、３級であった。但し、堅牢化処理における処理液のｐＨに起因すると思われる生地色のくすみが若干生じた。 When the chlorine fastness of the obtained polyphenol-treated cotton fabric was measured, it was grade 3. However, the fabric color was slightly dull, which may be caused by the pH of the treatment liquid in the fastening treatment.
（試料３）
精錬を行ったポリエステル生地１kgを、染浴中で約１５Ｌの水に浸し、十分に水を含浸させた。これに、カチオン剤（商品名：カチオノンＫＣＮ、一方社油脂工業社製４級アンモニウム塩）７０ｇを加えて１０分間攪拌した。更に、約３Ｌの水を追加して染浴中の液量を２０Ｌに調整し、加熱して５０℃まで昇温し、温度を維持して３０分間攪拌しながらポリエステル生地を十分に浸漬した。この後、染浴の液を排出し、流水で生地を念入りに水洗して中和しながら、洗浄水を排出した。
(Sample 3)
1 kg of the smelted polyester fabric was immersed in about 15 L of water in a dye bath and sufficiently impregnated with water. To this was added 70 g of a cation agent (trade name: Cationone KCN, quaternary ammonium salt manufactured by Yushi Kogyo Co., Ltd.) and stirred for 10 minutes. Further, about 3 L of water was added to adjust the amount of liquid in the dye bath to 20 L, heated to 50 ° C., and the polyester fabric was sufficiently immersed while stirring for 30 minutes while maintaining the temperature. Thereafter, the dyebath solution was discharged, and the washing water was discharged while the fabric was carefully washed with running water and neutralized.
染浴に約１５Ｌの水を投入してポリエステル生地を浸した。茶抽出ポリフェノール（商品名：テアフラン３０Ｆ、株式会社伊藤園製）１０ｇを約１Ｌの水に溶解して染浴に投入し、水を追加して染浴の液量を２０Ｌに調整した。これを加熱して５０℃まで昇温し、温度を維持して２０分間攪拌しながらポリエステル生地を十分に浸漬した。この後、染浴の液を排出して、流水でポリエステル生地を念入りに水洗し、生地を取り出して脱水、乾燥することにより、ポリフェノール加工ポリエステル布を得た。 About 15 L of water was poured into the dye bath to immerse the polyester fabric. 10 g of tea-extracted polyphenol (trade name: Theafuran 30F, manufactured by ITO EN Co., Ltd.) was dissolved in about 1 L of water and poured into the dye bath, and water was added to adjust the liquid volume of the dye bath to 20 L. This was heated up to 50 ° C., and the polyester fabric was sufficiently immersed while stirring for 20 minutes while maintaining the temperature. Thereafter, the dye bath was discharged, the polyester fabric was carefully washed with running water, the fabric was taken out, dehydrated and dried to obtain a polyphenol-treated polyester fabric.
上述で得たポリフェノール加工ポリエステル布について、耐光堅牢度及び塩素堅牢度を測定したところ、耐光堅牢度は３級、塩素堅牢度は２−３級であった。 When the light fastness and chlorine fastness of the polyphenol-treated polyester fabric obtained above were measured, the light fastness was grade 3 and the chlorine fastness was grade 2-3.
（試料３Ａ）
試料３で得たポリフェノール加工ポリエステル布１kgを、染浴中で約１５Ｌの水に浸し、十分に水を含浸させた。これに、分散性フェニルアミド処理剤（商品名：ＩＴＮ００３Ｍ、（株）竹内商店製アニオン性フェニルアミド系繊維加工剤、樹脂含有酸性水性液）２０ｇを添加して１０分間攪拌し、水を追加して染浴の液量を２０Ｌに調整した（ｐＨ６．７）。これを加熱して８０℃まで昇温し、温度を維持して３０分間攪拌しながらポリエステル生地を十分に浸漬した。この後、染浴の液を排出して、流水でポリエステル生地を念入りに水洗し、生地を取り出して脱水、乾燥することにより、フェニルアミド処理後のポリフェノール加工ポリエステル布を得た。
(Sample 3A)
1 kg of the polyphenol-treated polyester fabric obtained in Sample 3 was immersed in about 15 L of water in a dye bath and sufficiently impregnated with water. To this was added 20 g of a dispersible phenylamide treatment agent (trade name: ITN003M, an anionic phenylamide fiber processing agent manufactured by Takeuchi Shoten Co., Ltd., a resin-containing acidic aqueous solution), stirred for 10 minutes, and water was added. The amount of the dye bath was adjusted to 20 L (pH 6.7). This was heated and heated up to 80 ° C., and the polyester fabric was sufficiently immersed while stirring for 30 minutes while maintaining the temperature. Thereafter, the dye bath was discharged, the polyester fabric was carefully washed with running water, the fabric was taken out, dehydrated and dried to obtain a polyphenol-treated polyester fabric after phenylamide treatment.
得られたポリフェノール加工ポリエステル布について、耐光堅牢度及び塩素堅牢度を測定したところ、耐光堅牢度は３級、塩素堅牢度は３−４級であった。 When the light fastness and chlorine fastness of the obtained polyphenol-treated polyester fabric were measured, the light fastness was grade 3 and the chlorine fastness was grade 3-4.
（試料４）
精錬を行ったナイロン生地１kgを、染浴中で約１５Ｌの水に浸し、十分に水を含浸させた。茶抽出ポリフェノール（商品名：テアフラン３０Ｆ、株式会社伊藤園製）５ｇを約１Ｌの水に溶解して染浴に投入し、水を追加して染浴の液量を２０Ｌに調整した。これを加熱して８０℃まで昇温し、温度を維持して３０分間攪拌しながらナイロン生地を十分に浸漬した。この後、染浴の液を排出して、流水でナイロン生地を念入りに水洗し、生地を取り出して脱水、乾燥することにより、ポリフェノール加工ナイロン布を得た。
(Sample 4)
1 kg of the refined nylon fabric was immersed in about 15 L of water in a dye bath and sufficiently impregnated with water. 5 g of tea-extracted polyphenol (trade name: Teafuran 30F, manufactured by ITO EN Co., Ltd.) was dissolved in about 1 L of water and added to the dye bath, and water was added to adjust the amount of the dye bath to 20 L. This was heated to 80 ° C., and the nylon fabric was sufficiently immersed while stirring for 30 minutes while maintaining the temperature. Thereafter, the dye bath was discharged, the nylon fabric was carefully washed with running water, the fabric was taken out, dehydrated and dried to obtain a polyphenol-treated nylon fabric.
上述で得たポリフェノール加工ナイロン布について、塩素堅牢度を測定したところ、４級であった。 When the chlorine fastness of the polyphenol-treated nylon cloth obtained above was measured, it was grade 4.
（試料４Ａ）
精錬を行ったナイロン生地１kgを、染浴中で約１５Ｌの水に浸し、十分に水を含浸させた。茶抽出ポリフェノール（商品名：テアフラン３０Ｆ、株式会社伊藤園製）５ｇを約１Ｌの水に溶解して染浴に投入し、これを加熱して８０℃まで昇温し、分散性フェニルアミド処理剤（商品名：ＩＴＮ００３Ｍ、（株）竹内商店製アニオン性フェニルアミド系繊維加工剤、樹脂含有酸性水性液）３０ｇを添加して１０分間攪拌し、水を追加して染浴の液量を２０Ｌに調整した（ｐＨ６．７）。これを加熱して８０℃まで昇温し、温度を維持して３０分間攪拌しながらナイロン生地を十分に浸漬した。この後、染浴の液を排出して、流水でナイロン生地を念入りに水洗し、生地を取り出して脱水、乾燥することにより、フェニルアミド処理後のポリフェノール加工ナイロン布を得た。
(Sample 4A)
1 kg of the refined nylon fabric was immersed in about 15 L of water in a dye bath and sufficiently impregnated with water. 5 g of tea-extracted polyphenol (trade name: Theafuran 30F, manufactured by ITO EN Co., Ltd.) is dissolved in about 1 L of water and poured into a dyeing bath. Product Name: ITN003M, Takeuchi Shoten Anionic Phenylamide Fiber Finishing Agent, Resin-containing Acidic Aqueous Solution (30 g) is added and stirred for 10 minutes. Water is added to adjust the dye bath volume to 20 L. (PH 6.7). This was heated to 80 ° C., and the nylon fabric was sufficiently immersed while stirring for 30 minutes while maintaining the temperature. Thereafter, the dye bath was discharged, the nylon fabric was carefully washed with running water, the fabric was taken out, dehydrated and dried to obtain a polyphenol-treated nylon fabric after phenylamide treatment.
得られたポリフェノール加工ナイロン布について、塩素堅牢度を測定したところ、４級であった。 When the chlorine fastness of the obtained polyphenol-treated nylon cloth was measured, it was grade 4.
（試料５）
精錬漂白を行った綿生地１kgを、染浴中で約１５Ｌの水に浸し、十分に水を含浸させた。これに、カチオン剤（商品名：カチオノンＫＣＮ、一方社油脂工業社製４級アンモニウム塩）１００ｇを加えて１０分間攪拌した。更に、約１Ｌの水に水酸化ナトリウム２０ｇを溶解した溶液を調製して染浴に加え、１０分間攪拌した。約３Ｌの水を追加して染浴中の液量を２０Ｌに調整し、加熱して８０℃まで昇温し、温度を維持して３０分間攪拌しながら綿生地を十分に浸漬した。この後、染浴の液を排出し、流水で綿生地を念入りに水洗して中和しながら、洗浄水を排出した。
(Sample 5)
1 kg of cotton fabric subjected to refining and bleaching was immersed in about 15 L of water in a dyeing bath and sufficiently impregnated with water. To this was added 100 g of a cation agent (trade name: Cationone KCN, quaternary ammonium salt manufactured by Yushi Kogyo Co., Ltd.) and stirred for 10 minutes. Further, a solution in which 20 g of sodium hydroxide was dissolved in about 1 L of water was prepared, added to the dye bath, and stirred for 10 minutes. About 3 L of water was added to adjust the amount of liquid in the dye bath to 20 L, heated to 80 ° C., and the cotton fabric was sufficiently immersed while stirring for 30 minutes while maintaining the temperature. Thereafter, the dyebath solution was discharged, and the washing water was discharged while the cotton fabric was carefully washed with running water and neutralized.
染浴に約１５Ｌの水を投入して綿生地を浸した。ブドウポリフェノール５ｇを約１Ｌの水に溶解して染浴に投入し、水を追加して染浴の液量を２０Ｌに調整した。これを加熱して３０℃まで昇温し、温度を維持して２０分間攪拌しながら綿生地を十分に浸漬した。この後、染浴の液を排出して、流水で綿生地を念入りに水洗し、綿生地を取り出して脱水、乾燥することにより、ポリフェノール加工綿布を得た。 About 15 L of water was poured into the dye bath to immerse the cotton fabric. Grape polyphenol (5 g) was dissolved in about 1 L of water and poured into a dye bath, and water was added to adjust the amount of the dye bath to 20 L. This was heated and heated up to 30 ° C., and the cotton fabric was sufficiently immersed while stirring for 20 minutes while maintaining the temperature. Thereafter, the dyebath solution was discharged, the cotton fabric was carefully washed with running water, the cotton fabric was taken out, dehydrated and dried to obtain a polyphenol-treated cotton fabric.
上述で得たポリフェノール加工綿布について、塩素堅牢度を測定したところ、２級であった。 When the chlorine fastness of the polyphenol-treated cotton fabric obtained above was measured, it was second grade.
（試料５Ａ）
試料５で得たポリフェノール加工綿布１kgを、染浴中で約１５Ｌの水に浸し、十分に水を含浸させた。これに、分散性フェニルアミド処理剤（商品名：ＩＴＮ００３Ｍ、（株）竹内商店製アニオン性フェニルアミド系繊維加工剤、樹脂含有酸性水性液）２０ｇを添加して１０分間攪拌し、約４Ｌの水を追加して染浴の液量を２０Ｌに調整した（ｐＨ６．７）。これを加熱して５０℃まで昇温し、温度を維持して３０分間攪拌しながら綿生地を十分に浸漬した。この後、染浴の液を排出して、流水で綿生地を念入りに水洗し、綿生地を取り出して脱水、乾燥することにより、フェニルアミド処理後のポリフェノール加工綿布を得た。
(Sample 5A)
1 kg of the polyphenol-treated cotton fabric obtained in Sample 5 was immersed in about 15 L of water in a dye bath and sufficiently impregnated with water. To this, 20 g of a dispersible phenylamide treatment agent (trade name: ITN003M, an anionic phenylamide fiber processing agent manufactured by Takeuchi Shoten Co., Ltd., resin-containing acidic aqueous liquid) was added and stirred for 10 minutes, and about 4 L of water was added. Was added to adjust the amount of the dye bath to 20 L (pH 6.7). This was heated and heated up to 50 ° C., and the cotton fabric was sufficiently immersed while stirring for 30 minutes while maintaining the temperature. Thereafter, the dyebath solution was discharged, the cotton fabric was carefully washed with running water, the cotton fabric was taken out, dehydrated and dried to obtain a polyphenol-treated cotton fabric after phenylamide treatment.
得られたポリフェノール加工綿布について、塩素堅牢度を測定したところ、２−３級であった。 When the chlorine fastness of the obtained polyphenol-treated cotton fabric was measured, it was 2-3.
（試料６Ａ）
精錬漂白を行った綿生地を予め化学染料を用いて染色して染色綿生地を用意した。この染色綿生地１kgを、染浴中で約１５Ｌの水に浸し、十分に水を含浸させた。これに、茶抽出ポリフェノール（商品名：テアフラン３０Ｆ、株式会社伊藤園製）５ｇを約１Ｌの水に溶解して染浴に投入し、これを加熱して８０℃まで昇温した。錫酸ナトリウム１０ｇ及びクエン酸２０ｇを約１Ｌの水に溶解した水溶液を染浴に投入し、次いで、分散性フェニルアミド処理剤（商品名：ＩＴＮ００３Ｍ、（株）竹内商店製アニオン性フェニルアミド系繊維加工剤、樹脂含有酸性水性液）３０ｇを添加して（ｐＨ４．５）、８０℃で１０分間攪拌した。水を追加して染浴の液量を２０Ｌに調整して、８０℃で３０分間攪拌しながら綿生地を十分に浸漬した。この後、染浴の液を排出して、流水で綿生地を念入りに水洗し、綿生地を取り出して脱水、乾燥することにより、フェニルアミド処理したポリフェノール加工綿布を得た。
(Sample 6A)
A cotton fabric subjected to refining bleaching was previously dyed with a chemical dye to prepare a dyed cotton fabric. 1 kg of this dyed cotton fabric was immersed in about 15 L of water in a dye bath and sufficiently impregnated with water. To this, 5 g of tea-extracted polyphenol (trade name: Theafuran 30F, manufactured by ITO EN Co., Ltd.) was dissolved in about 1 L of water and poured into a dye bath, which was heated to 80 ° C. An aqueous solution obtained by dissolving 10 g of sodium stannate and 20 g of citric acid in about 1 L of water is put into a dyeing bath, and then a dispersible phenylamide treatment agent (trade name: ITN003M, anionic phenylamide fiber manufactured by Takeuchi Shoten Co., Ltd.) 30 g of processing agent and resin-containing acidic aqueous solution) were added (pH 4.5), and the mixture was stirred at 80 ° C. for 10 minutes. Water was added to adjust the dye bath volume to 20 L, and the cotton fabric was sufficiently immersed while stirring at 80 ° C. for 30 minutes. Thereafter, the dye bath was discharged, the cotton fabric was carefully washed with running water, the cotton fabric was taken out, dehydrated and dried to obtain a phenylamide-treated polyphenol-treated cotton fabric.
得られたポリフェノール加工綿布について、耐光堅牢度及び塩素堅牢度を測定したところ、耐光堅牢度は３級、塩素堅牢度は４−５級であった。 When the light fastness and chlorine fastness of the obtained polyphenol-treated cotton fabric were measured, the light fastness was grade 3 and the chlorine fastness was grade 4-5.
（試料７）
試料１で得たポリフェノール加工綿布１kgを、染浴中で約２０Ｌの水に浸し、十分に水を含浸させた。これに、市販の塩素堅牢度向上フィックス剤（商品名：モリロンＷＳ、モーリン化学工業株式会社製、アニオン性褐色液体）３０ｇを添加し、これを加熱して４０℃まで昇温し、温度を維持して１０分間攪拌しながら綿生地を十分に浸漬した。この後、染浴の液を排出して、流水で綿生地を念入りに水洗し、綿生地を取り出して脱水、乾燥することにより、フィックス剤処理後のポリフェノール加工綿布を得た。
(Sample 7)
1 kg of the polyphenol-treated cotton fabric obtained in Sample 1 was immersed in about 20 L of water in a dye bath and sufficiently impregnated with water. To this was added 30 g of a commercially available chlorine fastness-fixing agent (trade name: Morillon WS, manufactured by Morin Chemical Industry Co., Ltd., an anionic brown liquid), and this was heated to 40 ° C. to maintain the temperature. The cotton fabric was sufficiently immersed while stirring for 10 minutes. Thereafter, the dye bath was discharged, the cotton fabric was carefully washed with running water, the cotton fabric was taken out, dehydrated and dried to obtain a polyphenol-treated cotton fabric after the fixer treatment.
得られたポリフェノール加工綿布について、耐光堅牢度及び塩素堅牢度を測定したところ、耐光堅牢度は１級、塩素堅牢度は３級であった。 When the light fastness and the chlorine fastness of the obtained polyphenol-treated cotton fabric were measured, the light fastness was grade 1 and the chlorine fastness was grade 3.
（試料８）
試料１で得たポリフェノール加工綿布１kgを、染浴中で約２０Ｌの水に浸し、十分に水を含浸させた。これに、市販の塩素堅牢度向上フィックス剤（商品名：ダンフィックス５０００、日東紡株式会社製、カチオン性淡黄色酸性液体）３０ｇを添加し（ｐＨ４．０）、これを加熱して４０℃まで昇温し、温度を維持して１０分間攪拌しながら綿生地を十分に浸漬した。この後、染浴の液を排出して、流水で綿生地を念入りに水洗し、綿生地を取り出して脱水、乾燥することにより、フィックス剤処理後のポリフェノール加工綿布を得た。
(Sample 8)
1 kg of the polyphenol-treated cotton fabric obtained in Sample 1 was immersed in about 20 L of water in a dye bath and sufficiently impregnated with water. To this was added 30 g of a commercially available chlorine fastness improving fix agent (trade name: Dunfix 5000, manufactured by Nittobo Co., Ltd., a cationic light yellow acidic liquid) (pH 4.0), and this was heated to 40 ° C. The temperature was raised and the cotton fabric was sufficiently immersed while stirring for 10 minutes while maintaining the temperature. Thereafter, the dye bath was discharged, the cotton fabric was carefully washed with running water, the cotton fabric was taken out, dehydrated and dried to obtain a polyphenol-treated cotton fabric after the fixer treatment.
得られたポリフェノール加工綿布について、耐光堅牢度及び塩素堅牢度を測定したところ、耐光堅牢度は３級、塩素堅牢度は３級であった。但し、フィックス剤の酸に起因すると考えられるポリフェノールの脱色が生じた。 When the light fastness and chlorine fastness of the obtained polyphenol-treated cotton fabric were measured, the light fastness was grade 3 and the chlorine fastness was grade 3. However, the decolorization of polyphenol considered to be caused by the acid of the fixing agent occurred.
（試料９）
試料１で得たポリフェノール加工綿布１kgを、染浴中で約２０Ｌの水に浸し、十分に水を含浸させた。これに、市販の塩素堅牢度向上フィックス剤（商品名：ダンフィックス７０００、日東紡株式会社製、カチオン性淡黄色アルカリ性液体）３０ｇを添加し（ｐＨ８．０）、これを加熱して４０℃まで昇温し、温度を維持して１０分間攪拌しながら綿生地を十分に浸漬した。この後、染浴の液を排出して、流水で綿生地を念入りに水洗し、綿生地を取り出して脱水、乾燥することにより、フィックス剤処理後のポリフェノール加工綿布を得た。
(Sample 9)
1 kg of the polyphenol-treated cotton fabric obtained in Sample 1 was immersed in about 20 L of water in a dye bath and sufficiently impregnated with water. To this was added 30 g of a commercially available chlorine fastness-fixing agent (trade name: Dunfix 7000, manufactured by Nittobo Co., Ltd., a cationic light yellow alkaline liquid) (pH 8.0), and this was heated to 40 ° C. The temperature was raised and the cotton fabric was sufficiently immersed while stirring for 10 minutes while maintaining the temperature. Thereafter, the dye bath was discharged, the cotton fabric was carefully washed with running water, the cotton fabric was taken out, dehydrated and dried to obtain a polyphenol-treated cotton fabric after the fixer treatment.
得られたポリフェノール加工綿布について、耐光堅牢度及び塩素堅牢度を測定したところ、耐光堅牢度は３級、塩素堅牢度は３級であった。但し、フィックス剤のアルカリに起因すると考えられるポリフェノールの色くすみが生じた。 When the light fastness and chlorine fastness of the obtained polyphenol-treated cotton fabric were measured, the light fastness was grade 3 and the chlorine fastness was grade 3. However, the color haze of polyphenol considered to be caused by the alkali of the fixing agent occurred.
（試料１０）
精錬漂白を行った綿生地１kgを、染浴中で約１５Ｌの水に浸し、十分に水を含浸させた。これに、茶抽出ポリフェノール（商品名：テアフラン３０Ｆ、株式会社伊藤園製）５ｇを約１Ｌの水に溶解して投入し、これを加熱して８０℃まで昇温した。錫酸ナトリウム１０ｇ及びクエン酸２０ｇを約１Ｌの水に溶解した水溶液を染浴に投入し、水を追加して染浴の液量を２０Ｌに調整して、８０℃で１０分間攪拌しながら綿生地を十分に浸漬した。これに、水溶性フェニルアミド処理剤（商品名：アモルデンＭＣＭ−４００、大和化学株式会社製アニオン性フェニルアミド系繊維加工剤、酸性水性液）３０ｇを添加して（ｐＨ６．５）、８０℃で３０分間攪拌した。この後、染浴の液を排出して、流水で綿生地を念入りに水洗し、綿生地を取り出して脱水、乾燥することにより、ポリフェノール加工綿布を得た。
(Sample 10)
1 kg of cotton fabric subjected to refining and bleaching was immersed in about 15 L of water in a dyeing bath and sufficiently impregnated with water. To this, 5 g of tea-extracted polyphenol (trade name: Teafuran 30F, manufactured by ITO EN Co., Ltd.) was dissolved in about 1 L of water, and this was heated and heated to 80 ° C. An aqueous solution obtained by dissolving 10 g of sodium stannate and 20 g of citric acid in about 1 L of water is added to the dyeing bath, water is added to adjust the amount of the dyeing bath to 20 L, and cotton is stirred at 80 ° C. for 10 minutes. The dough was fully immersed. To this was added 30 g of a water-soluble phenylamide treatment agent (trade name: Amorden MCM-400, anionic phenylamide fiber processing agent, acidic aqueous liquid manufactured by Daiwa Chemical Co., Ltd.) (pH 6.5), and at 80 ° C. Stir for 30 minutes. Thereafter, the dyebath solution was discharged, the cotton fabric was carefully washed with running water, the cotton fabric was taken out, dehydrated and dried to obtain a polyphenol-treated cotton fabric.
得られたポリフェノール加工綿布について、塩素堅牢度を測定したところ、３級基準を満たさず、塩素堅牢度の向上は見られなかった。 When the chlorine fastness of the obtained polyphenol-treated cotton fabric was measured, the grade 3 standard was not satisfied, and no improvement in the chlorine fastness was observed.
（試料１１）
精錬漂白を行った綿生地１kgを、染浴中で約１５Ｌの水に浸し、十分に水を含浸させた。これに、茶抽出ポリフェノール（商品名：テアフラン３０Ｆ、株式会社伊藤園製）５ｇを約１Ｌの水に溶解して投入し、これを加熱して８０℃まで昇温した。錫酸ナトリウム１０ｇ及びクエン酸２０ｇを約１Ｌの水に溶解した水溶液を染浴に投入し、水を追加して染浴の液量を２０Ｌに調整して、８０℃で１０分間攪拌しながら綿生地を十分に浸漬した。これに、分散性アクリル樹脂系処理剤（商品名：ファイコートＮ−１２５、大和化学株式会社製アニオン性アクリル樹脂系繊維加工剤、弱酸性液）３０ｇを添加して（ｐＨ５．０）、８０℃で３０分間攪拌した。この後、染浴の液を排出して、流水で綿生地を念入りに水洗し、綿生地を取り出して脱水、乾燥することにより、ポリフェノール加工綿布を得た。
(Sample 11)
1 kg of cotton fabric subjected to refining and bleaching was immersed in about 15 L of water in a dyeing bath and sufficiently impregnated with water. To this, 5 g of tea-extracted polyphenol (trade name: Teafuran 30F, manufactured by ITO EN Co., Ltd.) was dissolved in about 1 L of water, and this was heated and heated to 80 ° C. An aqueous solution obtained by dissolving 10 g of sodium stannate and 20 g of citric acid in about 1 L of water is added to the dyeing bath, water is added to adjust the amount of the dyeing bath to 20 L, and cotton is stirred at 80 ° C. for 10 minutes. The dough was fully immersed. To this, 30 g of a dispersible acrylic resin-based treatment agent (trade name: Phicoat N-125, an anionic acrylic resin-based fiber processing agent manufactured by Daiwa Chemical Co., Ltd., weakly acidic liquid) was added (pH 5.0), 80 Stir at 30 ° C. for 30 minutes. Thereafter, the dyebath solution was discharged, the cotton fabric was carefully washed with running water, the cotton fabric was taken out, dehydrated and dried to obtain a polyphenol-treated cotton fabric.
得られたポリフェノール加工綿布について、塩素堅牢度を測定したところ、３級基準を満たさず、塩素堅牢度の向上は見られなかった。 When the chlorine fastness of the obtained polyphenol-treated cotton fabric was measured, the grade 3 standard was not satisfied, and no improvement in the chlorine fastness was observed.
（ポリフェノール加工繊維の物性及び機能性）
試料２Ａで得られた堅牢化処理後のポリフェノール加工綿布について、各種堅牢度、抗菌性、消臭性、紫外線遮蔽能、抗酸化性、安全性を調べた。結果を下記の表１に示す。
(Physical properties and functionality of polyphenol processed fiber)
Various fastnesses, antibacterial properties, deodorizing properties, ultraviolet shielding ability, antioxidant properties, and safety were examined for the fastened polyphenol-treated cotton fabric obtained in Sample 2A. The results are shown in Table 1 below.
（表１）
ポリフェノール加工繊維（試料２Ａ）の物性及び機能性
堅牢度
洗濯堅牢度（JIS L0844 A-2号）：（変退色）５級、（汚染）５級
汗堅牢度（JIS L0848）：（酸性変退色）５級、（酸性汚染）５級、
（塩基性変退色）５級、（塩基性汚染）５級
摩擦堅牢度（JIS L0849 摩擦試験機II型）：（乾燥）５級、（湿潤）５級
抗菌性（JIS L1902 黄色ブドウ球菌を用いた菌液吸収法）
製造直後：生菌数＜８．３×１０３、静菌活性値＞３．１、制菌活性値＞０．４
洗濯10回後：生菌数＜８．３×１０３、静菌活性値＞３．１、制菌活性値＞０．４
（綿標準白布の生菌数）
接種直後生菌数：２．０×１０ ４ 、１８時間後生菌数：１．１×１０ ７ ）
消臭性（JAFET基準試験方法）
アンモニア（検知管法）：８６．３％
酢酸（検知管法）：８８．０％
イソ吉草酸（ガスクロ法）：９８．０％
紫外線遮蔽能（測定波長：２８０〜４００nm）
試料２：（平均遮蔽率）７０．６％、（ＵＰＦ値）７．４
試料２Ａ：（平均遮蔽率）７９．３％、（ＵＰＦ値）１０．２
抗酸化性（リノール酸を用いたＣＤＭ試験で酸化が始まるまでの時間）
ブランク：７．５時間
未加工綿布：８．０時間
試料２Ａ：９．７時間
安全性：河合法皮膚貼付試験
試験結果：２Ｂ、判定：準陰性
安全性：溶出試験（エコテックススタンダード１００ クラスＩ溶出試験）
Ｓｂ：１．０２ppm、Ａｓ：n/d、Ｐｂ：n/d、Ｃｄ：n/d、Ｃｒ：n/d、
Ｃｒ(VI)：n/d、Ｃｏ：n/d、Ｃｕ：５．２４ppm、Ｎｉ：n/d、Ｈｇ：n/d、
農薬：n/d
(Table 1)
Physical properties and functionality of polyphenol processed fiber (Sample 2A)
Fastness Washing fastness (JIS L0844 A-2): (discoloration) grade 5, (contamination) grade 5 Sweat fastness (JIS L0848): (acid discoloration) grade 5, (acid pollution) grade 5,
(Basic discoloration) Grade 5, (Basic contamination) Grade 5
Friction fastness (JIS L0849 Friction Tester Type II): (Dry) Grade 5 (Wet) Grade 5
Antibacterial (bacteria absorption method using JIS L1902 Staphylococcus aureus)
Immediately after production: viable cell count <8.3 × 10 3 , bacteriostatic activity value> 3.1, bacteriostatic activity value> 0.4
After 10 washings: Viable count <8.3 × 10 3 , bacteriostatic activity value> 3.1, bactericidal activity value> 0.4
(Viable bacteria count of cotton standard white cloth)
Number of viable bacteria immediately after inoculation: 2.0 × 10 4 , number of viable bacteria after 18 hours: 1.1 × 10 7 )
Deodorant (JAFET standard test method)
Ammonia (detector tube method): 86.3%
Acetic acid (detector tube method): 88.0%
Isovaleric acid (gas chromatographic method): 98.0%
UV shielding ability (measurement wavelength: 280-400 nm)
Sample 2: (Average shielding factor) 70.6%, (UPF value) 7.4
Sample 2A: (average shielding rate) 79.3%, (UPF value) 10.2.
Antioxidant (Time until oxidation starts in CDM test using linoleic acid)
Blank: 7.5 hours Raw cotton: 8.0 hours
Sample 2A: 9.7 hours
Safety: Kawai skin patch test Test result: 2B, Judgment: Semi-negative Safety: Dissolution test (Ecotex Standard 100 class I dissolution test)
Sb: 1.02 ppm, As: n / d, Pb: n / d, Cd: n / d, Cr: n / d,
Cr (VI): n / d, Co: n / d, Cu: 5.24 ppm, Ni: n / d, Hg: n / d,
Pesticide: n / d
表１から明らかなように、分散性フェニルアミドを用いた堅牢化処理をポリフェノール加工繊維に施すことによって、洗濯堅牢度や汗堅牢度、摩擦堅牢度が低下することはなく、ポリフェノールの機能性である抗菌性、消臭性、抗酸化性も保持され、紫外線遮蔽能も向上する。又、身体や環境に対する安全性も保持している。 As is clear from Table 1, by applying a fastening treatment using dispersible phenylamide to the polyphenol-processed fiber, the fastness to washing, the fastness to sweat, and the fastness to friction are not reduced. Certain antibacterial properties, deodorant properties, and antioxidant properties are also maintained, and the ultraviolet shielding ability is improved. It also maintains safety for the body and the environment.
ポリフェノールの染色性や機能を損なうことなく、ポリフェノール加工繊維の耐光堅牢度を保持したまま塩素堅牢度を改善することができるので、一般衣類や服飾品、布地を用いた台所用品、装飾品、アメニティ製品等の様々な繊維利用製品に幅広く適用して高品質の製品を提供することができ、ポリフェノールの機能性を利用した製品の用途開発を促進することができる。従って、ポリフェノール加工繊維製品の普及に有用である。 The chlorine fastness can be improved while maintaining the light fastness of the polyphenol-processed fiber without impairing the dyeability and function of the polyphenol, so that it can be used for general clothing and clothing, kitchen utensils using fabrics, ornaments, and amenities. It can be widely applied to various fiber-utilizing products such as products to provide high-quality products, and the use development of products utilizing the functionality of polyphenols can be promoted. Therefore, it is useful for the spread of polyphenol processed fiber products.
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| JP6892674B2 (en) * | 2016-12-09 | 2021-06-23 | おぼろタオル株式会社 | Textile products and manufacturing methods for textile products |
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