JP5159534B2 - Water permeability imparting agent, water permeable fiber to which it is attached, and method for producing nonwoven fabric - Google Patents
Water permeability imparting agent, water permeable fiber to which it is attached, and method for producing nonwoven fabric Download PDFInfo
- Publication number
- JP5159534B2 JP5159534B2 JP2008238893A JP2008238893A JP5159534B2 JP 5159534 B2 JP5159534 B2 JP 5159534B2 JP 2008238893 A JP2008238893 A JP 2008238893A JP 2008238893 A JP2008238893 A JP 2008238893A JP 5159534 B2 JP5159534 B2 JP 5159534B2
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- Prior art keywords
- water
- component
- imparting agent
- carbon atoms
- group
- Prior art date
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims description 159
- 230000035699 permeability Effects 0.000 title claims description 131
- 239000003795 chemical substances by application Substances 0.000 title claims description 101
- 239000000835 fiber Substances 0.000 title claims description 99
- 239000004745 nonwoven fabric Substances 0.000 title claims description 46
- 238000004519 manufacturing process Methods 0.000 title claims description 24
- -1 alkyl phosphate salt Chemical class 0.000 claims description 91
- 125000004432 carbon atom Chemical group C* 0.000 claims description 73
- 235000014113 dietary fatty acids Nutrition 0.000 claims description 43
- 229930195729 fatty acid Natural products 0.000 claims description 43
- 239000000194 fatty acid Substances 0.000 claims description 43
- 238000000034 method Methods 0.000 claims description 42
- 125000000217 alkyl group Chemical group 0.000 claims description 30
- 150000002148 esters Chemical class 0.000 claims description 28
- OFOBLEOULBTSOW-UHFFFAOYSA-N Malonic acid Chemical compound OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 claims description 22
- 125000001931 aliphatic group Chemical group 0.000 claims description 21
- 150000004665 fatty acids Chemical class 0.000 claims description 21
- 150000001875 compounds Chemical class 0.000 claims description 20
- 150000005846 sugar alcohols Polymers 0.000 claims description 19
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 17
- 229910052799 carbon Inorganic materials 0.000 claims description 16
- 229920000098 polyolefin Polymers 0.000 claims description 15
- 239000002280 amphoteric surfactant Substances 0.000 claims description 14
- 125000001183 hydrocarbyl group Chemical group 0.000 claims description 13
- 125000002947 alkylene group Chemical group 0.000 claims description 9
- 239000004094 surface-active agent Substances 0.000 claims description 9
- 239000003093 cationic surfactant Substances 0.000 claims description 8
- 150000003839 salts Chemical class 0.000 claims description 8
- 125000004435 hydrogen atom Chemical group [H]* 0.000 claims description 4
- 125000002768 hydroxyalkyl group Chemical group 0.000 claims description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 claims description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical group [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 3
- KKUKTXOBAWVSHC-UHFFFAOYSA-N Dimethylphosphate Chemical compound COP(O)(=O)OC KKUKTXOBAWVSHC-UHFFFAOYSA-N 0.000 claims description 3
- KIWBPDUYBMNFTB-UHFFFAOYSA-N Ethyl hydrogen sulfate Chemical compound CCOS(O)(=O)=O KIWBPDUYBMNFTB-UHFFFAOYSA-N 0.000 claims description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 3
- NPYPAHLBTDXSSS-UHFFFAOYSA-N Potassium ion Chemical group [K+] NPYPAHLBTDXSSS-UHFFFAOYSA-N 0.000 claims description 3
- FKNQFGJONOIPTF-UHFFFAOYSA-N Sodium cation Chemical compound [Na+] FKNQFGJONOIPTF-UHFFFAOYSA-N 0.000 claims description 3
- ZBCBWPMODOFKDW-UHFFFAOYSA-O bis(2-hydroxyethyl)azanium Chemical group OCC[NH2+]CCO ZBCBWPMODOFKDW-UHFFFAOYSA-O 0.000 claims description 3
- 125000000816 ethylene group Chemical group [H]C([H])([*:1])C([H])([H])[*:2] 0.000 claims description 3
- 229910052736 halogen Inorganic materials 0.000 claims description 3
- 239000001257 hydrogen Substances 0.000 claims description 3
- 229910052739 hydrogen Inorganic materials 0.000 claims description 3
- GPRLSGONYQIRFK-UHFFFAOYSA-N hydron Chemical compound [H+] GPRLSGONYQIRFK-UHFFFAOYSA-N 0.000 claims description 3
- JZMJDSHXVKJFKW-UHFFFAOYSA-M methyl sulfate(1-) Chemical compound COS([O-])(=O)=O JZMJDSHXVKJFKW-UHFFFAOYSA-M 0.000 claims description 3
- 229910001414 potassium ion Inorganic materials 0.000 claims description 3
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 claims description 3
- 229910001415 sodium ion Inorganic materials 0.000 claims description 3
- GSEJCLTVZPLZKY-UHFFFAOYSA-O triethanolammonium Chemical group OCC[NH+](CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-O 0.000 claims description 3
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 2
- 125000004429 atom Chemical group 0.000 claims description 2
- 230000000903 blocking effect Effects 0.000 claims description 2
- 229940085991 phosphate ion Drugs 0.000 claims description 2
- 238000012545 processing Methods 0.000 claims description 2
- 239000007788 liquid Substances 0.000 description 35
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 17
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 13
- 230000002265 prevention Effects 0.000 description 12
- 229920001296 polysiloxane Polymers 0.000 description 10
- 229920005989 resin Polymers 0.000 description 10
- 239000011347 resin Substances 0.000 description 10
- 238000011156 evaluation Methods 0.000 description 9
- 238000004804 winding Methods 0.000 description 9
- UKMSUNONTOPOIO-UHFFFAOYSA-N docosanoic acid Chemical compound CCCCCCCCCCCCCCCCCCCCCC(O)=O UKMSUNONTOPOIO-UHFFFAOYSA-N 0.000 description 8
- 239000002504 physiological saline solution Substances 0.000 description 8
- 238000001035 drying Methods 0.000 description 7
- 239000000463 material Substances 0.000 description 7
- 239000004743 Polypropylene Substances 0.000 description 6
- 239000002131 composite material Substances 0.000 description 6
- 230000007423 decrease Effects 0.000 description 6
- 230000008034 disappearance Effects 0.000 description 6
- POULHZVOKOAJMA-UHFFFAOYSA-N dodecanoic acid Chemical compound CCCCCCCCCCCC(O)=O POULHZVOKOAJMA-UHFFFAOYSA-N 0.000 description 6
- 229920001155 polypropylene Polymers 0.000 description 6
- 238000010438 heat treatment Methods 0.000 description 5
- 229920001903 high density polyethylene Polymers 0.000 description 5
- 239000004700 high-density polyethylene Substances 0.000 description 5
- 230000000704 physical effect Effects 0.000 description 5
- 229920000139 polyethylene terephthalate Polymers 0.000 description 5
- 239000005020 polyethylene terephthalate Substances 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- 235000021357 Behenic acid Nutrition 0.000 description 4
- KWIUHFFTVRNATP-UHFFFAOYSA-N Betaine Natural products C[N+](C)(C)CC([O-])=O KWIUHFFTVRNATP-UHFFFAOYSA-N 0.000 description 4
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 4
- KWIUHFFTVRNATP-UHFFFAOYSA-O N,N,N-trimethylglycinium Chemical compound C[N+](C)(C)CC(O)=O KWIUHFFTVRNATP-UHFFFAOYSA-O 0.000 description 4
- 235000021355 Stearic acid Nutrition 0.000 description 4
- 229940116226 behenic acid Drugs 0.000 description 4
- 229960003237 betaine Drugs 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 231100000263 cytotoxicity test Toxicity 0.000 description 4
- WZPRPGQIPUCXQE-UHFFFAOYSA-L dipotassium;decyl phosphate Chemical compound [K+].[K+].CCCCCCCCCCOP([O-])([O-])=O WZPRPGQIPUCXQE-UHFFFAOYSA-L 0.000 description 4
- GWTCIAGIKURVBJ-UHFFFAOYSA-L dipotassium;dodecyl phosphate Chemical compound [K+].[K+].CCCCCCCCCCCCOP([O-])([O-])=O GWTCIAGIKURVBJ-UHFFFAOYSA-L 0.000 description 4
- LPZZAIMVFFLHQU-UHFFFAOYSA-L dipotassium;octyl phosphate Chemical compound [K+].[K+].CCCCCCCCOP([O-])([O-])=O LPZZAIMVFFLHQU-UHFFFAOYSA-L 0.000 description 4
- 230000007794 irritation Effects 0.000 description 4
- 235000019388 lanolin Nutrition 0.000 description 4
- VZCYOOQTPOCHFL-UPHRSURJSA-N maleic acid Chemical compound OC(=O)\C=C/C(O)=O VZCYOOQTPOCHFL-UPHRSURJSA-N 0.000 description 4
- 239000011976 maleic acid Substances 0.000 description 4
- 238000002844 melting Methods 0.000 description 4
- 230000008018 melting Effects 0.000 description 4
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 4
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 description 4
- 239000008117 stearic acid Substances 0.000 description 4
- 230000002195 synergetic effect Effects 0.000 description 4
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 description 4
- WCOXQTXVACYMLM-UHFFFAOYSA-N 2,3-bis(12-hydroxyoctadecanoyloxy)propyl 12-hydroxyoctadecanoate Chemical compound CCCCCCC(O)CCCCCCCCCCC(=O)OCC(OC(=O)CCCCCCCCCCC(O)CCCCCC)COC(=O)CCCCCCCCCCC(O)CCCCCC WCOXQTXVACYMLM-UHFFFAOYSA-N 0.000 description 3
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 3
- IAYPIBMASNFSPL-UHFFFAOYSA-N Ethylene oxide Chemical compound C1CO1 IAYPIBMASNFSPL-UHFFFAOYSA-N 0.000 description 3
- 239000004166 Lanolin Substances 0.000 description 3
- 239000005639 Lauric acid Substances 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 3
- KDYFGRWQOYBRFD-UHFFFAOYSA-N Succinic acid Natural products OC(=O)CCC(O)=O KDYFGRWQOYBRFD-UHFFFAOYSA-N 0.000 description 3
- ULUAUXLGCMPNKK-UHFFFAOYSA-N Sulfobutanedioic acid Chemical class OC(=O)CC(C(O)=O)S(O)(=O)=O ULUAUXLGCMPNKK-UHFFFAOYSA-N 0.000 description 3
- 230000002745 absorbent Effects 0.000 description 3
- 239000002250 absorbent Substances 0.000 description 3
- 239000006096 absorbing agent Substances 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 3
- 239000007864 aqueous solution Substances 0.000 description 3
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 3
- 238000009960 carding Methods 0.000 description 3
- CNXJITYCNQNTBD-UHFFFAOYSA-L dipotassium;hexadecyl phosphate Chemical compound [K+].[K+].CCCCCCCCCCCCCCCCOP([O-])([O-])=O CNXJITYCNQNTBD-UHFFFAOYSA-L 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000005304 joining Methods 0.000 description 3
- 229940039717 lanolin Drugs 0.000 description 3
- 229920001684 low density polyethylene Polymers 0.000 description 3
- 239000004702 low-density polyethylene Substances 0.000 description 3
- 238000005461 lubrication Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 229920000728 polyester Polymers 0.000 description 3
- 229920005672 polyolefin resin Polymers 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 description 2
- ULQISTXYYBZJSJ-UHFFFAOYSA-N 12-hydroxyoctadecanoic acid Chemical compound CCCCCCC(O)CCCCCCCCCCC(O)=O ULQISTXYYBZJSJ-UHFFFAOYSA-N 0.000 description 2
- KIHBGTRZFAVZRV-UHFFFAOYSA-N 2-Hydroxyoctadecanoic acid Natural products CCCCCCCCCCCCCCCCC(O)C(O)=O KIHBGTRZFAVZRV-UHFFFAOYSA-N 0.000 description 2
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 description 2
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 2
- 239000005642 Oleic acid Substances 0.000 description 2
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 description 2
- 229910019142 PO4 Inorganic materials 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 238000007259 addition reaction Methods 0.000 description 2
- WNLRTRBMVRJNCN-UHFFFAOYSA-N adipic acid Chemical compound OC(=O)CCCCC(O)=O WNLRTRBMVRJNCN-UHFFFAOYSA-N 0.000 description 2
- 239000003242 anti bacterial agent Substances 0.000 description 2
- YSJGOMATDFSEED-UHFFFAOYSA-M behentrimonium chloride Chemical compound [Cl-].CCCCCCCCCCCCCCCCCCCCCC[N+](C)(C)C YSJGOMATDFSEED-UHFFFAOYSA-M 0.000 description 2
- WPYMKLBDIGXBTP-UHFFFAOYSA-N benzoic acid Chemical compound OC(=O)C1=CC=CC=C1 WPYMKLBDIGXBTP-UHFFFAOYSA-N 0.000 description 2
- 210000001124 body fluid Anatomy 0.000 description 2
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- 239000004359 castor oil Substances 0.000 description 2
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- REZZEXDLIUJMMS-UHFFFAOYSA-M dimethyldioctadecylammonium chloride Chemical compound [Cl-].CCCCCCCCCCCCCCCCCC[N+](C)(C)CCCCCCCCCCCCCCCCCC REZZEXDLIUJMMS-UHFFFAOYSA-M 0.000 description 2
- 239000004664 distearyldimethylammonium chloride (DHTDMAC) Substances 0.000 description 2
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- IPCSVZSSVZVIGE-UHFFFAOYSA-N hexadecanoic acid Chemical compound CCCCCCCCCCCCCCCC(O)=O IPCSVZSSVZVIGE-UHFFFAOYSA-N 0.000 description 2
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- XAEFZNCEHLXOMS-UHFFFAOYSA-M potassium benzoate Chemical compound [K+].[O-]C(=O)C1=CC=CC=C1 XAEFZNCEHLXOMS-UHFFFAOYSA-M 0.000 description 2
- WBHHMMIMDMUBKC-XLNAKTSKSA-N ricinelaidic acid Chemical compound CCCCCC[C@@H](O)C\C=C\CCCCCCCC(O)=O WBHHMMIMDMUBKC-XLNAKTSKSA-N 0.000 description 2
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- 159000000000 sodium salts Chemical class 0.000 description 2
- RPACBEVZENYWOL-XFULWGLBSA-M sodium;(2r)-2-[6-(4-chlorophenoxy)hexyl]oxirane-2-carboxylate Chemical compound [Na+].C=1C=C(Cl)C=CC=1OCCCCCC[C@]1(C(=O)[O-])CO1 RPACBEVZENYWOL-XFULWGLBSA-M 0.000 description 2
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Description
本発明は、透水性付与剤、それが付着した透水性繊維および不織布の製造方法に関する。詳細には、不織布製造用ポリオレフィン系繊維に対して、本発明の透水性付与剤を付与することにより、不織布製造時のカード工程で優れた通過性が得られ、得られた不織布に瞬時透水性、耐久透水性、液戻り防止性を併せ持ち、かつ安全性にも優れる透水性付与剤、それが付着した透水性繊維および不織布の製造方法に関する。 The present invention relates to a water permeability imparting agent, a water permeable fiber to which it is attached, and a method for producing a nonwoven fabric. More specifically, by imparting the water permeability-imparting agent of the present invention to the polyolefin fiber for nonwoven fabric production, excellent permeability is obtained in the card process during the production of the nonwoven fabric, and the resulting nonwoven fabric has instant water permeability. Further, the present invention relates to a water permeability-imparting agent that has both durable water permeability and liquid return prevention properties, and is excellent in safety, and a method for producing water-permeable fibers and nonwoven fabrics to which the water-permeability imparting agent is attached.
一般に、紙おむつや合成ナプキンを代表とする生理用品等の吸収性物品は、疎水性の強いポリオレフィン系繊維、ポリエステル系繊維を主材とする各種不織布に親水性を付与したトップシートと、吸収材及び撥水性を付与したバックシートの間に綿状パルプや高分子吸収体等からなる材料を配置した３層から形成される構造になっている。尿や体液等の液体はトップシートを通過して吸収体に吸収されるが、この時トップシートのベトツキ感を無くすために、透水性のよいこと、すなわち液体がトップシート上から内部の吸収体に完全に吸収される迄の時間が極めて短い瞬時透水性が必要である。加えて一度吸収体に吸収された液体が再びトップシート上に戻らないようにすること、すなわち液戻り防止性が必要になる。さらに、僅か１回から２回の液体の吸収によってトップシート上の処理剤が流出して透水性が急激に低下するのは、おむつの取り替え回数が増すことになって好ましくないので、トップシートには繰り返しの液体吸収に耐える耐久透水性が要求される。また、不織布の製造面からはカード工程の高速化に伴いシリンダーへの巻付きやスカムが発生しないこと、すなわち良好なカード通過性が要求される。さらに、安全性への配慮から皮膚への刺激性の少ない要求が一層強くなってきている。親水性に極めて劣るポリオレフィン系繊維について、上記のような要求に応える透水性付与剤およびそれが付着した透水性繊維が要求されている。 In general, absorbent articles such as sanitary products such as disposable diapers and synthetic napkins are composed of top sheets made of hydrophilic materials such as polyolefin fibers and polyester fibers, which have strong hydrophobic properties, and absorbent materials. It has a structure formed of three layers in which a material made of cotton-like pulp, a polymer absorber, or the like is disposed between water-repellent backsheets. Liquids such as urine and body fluid pass through the top sheet and are absorbed by the absorber. At this time, in order to eliminate the sticky feeling of the top sheet, it is good in water permeability, that is, the liquid is absorbed from the top sheet to the internal absorber. Instantaneous water permeability is required which requires a very short time for complete absorption. In addition, it is necessary to prevent the liquid once absorbed by the absorbent body from returning to the top sheet again, that is, to prevent liquid return. Furthermore, it is not preferable that the treatment agent on the top sheet flows out due to absorption of the liquid only once or twice and the water permeability decreases rapidly, because this increases the number of diaper replacements. Is required to have durable water permeability to withstand repeated liquid absorption. Further, from the production side of the nonwoven fabric, it is required that the winding of the cylinder and the scum do not occur as the card process speeds up, that is, good card passing property is required. Furthermore, the demand for less irritation to the skin has become stronger due to safety considerations. For polyolefin fibers that are extremely inferior in hydrophilicity, a water-permeability imparting agent that meets the above requirements and a water-permeable fiber to which it adheres are required.
紙おむつの快適な着用のためには瞬時透水性がよく、繰り返しの透水に対しても透水性を維持し、且つ液戻り性を少なくすることが重要である。また不織布の製造時にはカード工程通過性が重要である。これらの特性を透水性付与剤によって改善する技術が提案されている。ポリオレフィン系繊維の疎水性繊維の表面に対して、瞬時透水性がよく、かつ繰り返しの液体透水に対しても透水性を維持するという相反する要求特性を透水性付与剤に求められ、アルキルホスフェート塩とカチオン性界面活性剤および両性界面活性剤等の配合割合の調整等で補っていた。しかし、瞬時透水性が得られる場合でも耐久透水性が不足したり、耐久透水性がある程度得られる場合でも瞬時透水性が不足したりして、現在の衛生材料用途に要求される瞬時透水性・耐久透水性の両者を満足するものが得られていなかった。さらには、皮膚への刺激性の強いものが多いという問題点があった。また、これらの成分に変性シリコーンを併用すると耐久透水性は少し改善されるものの、それでも不十分な性能レベルにあった。また、変性シリコーンを使用することにより液戻り防止性が不十分になったり、不織布の製造工程であるカード工程においてカード機にスカムが発生する問題があった。 For comfortable wearing of a disposable diaper, it is important to have instant water permeability, maintain water permeability even with repeated water permeability, and reduce liquid return. Further, the card process passability is important when manufacturing the nonwoven fabric. Techniques have been proposed for improving these characteristics with water permeability imparting agents. Alkyl phosphate salts are required for water permeability-imparting agents to have contradictory requirements for water permeability to the surface of hydrophobic fibers of polyolefin fibers and to maintain water permeability even for repeated liquid water permeability. And adjustment of the blending ratio of the cationic surfactant and the amphoteric surfactant. However, even when instantaneous water permeability is obtained, durable water permeability is insufficient, or even when durable water permeability is obtained to some extent, instantaneous water permeability is insufficient. A product satisfying both durable water permeability was not obtained. Furthermore, there was a problem that there were many things with strong irritation to skin. Further, when the modified silicone is used in combination with these components, the durable water permeability is slightly improved, but it is still at an insufficient performance level. In addition, the use of the modified silicone has a problem in that the anti-return property is insufficient, and scum is generated in the card machine in the card process, which is a process for manufacturing a nonwoven fabric.
たとえば、特許文献１ではアルキル燐酸エステル塩にポリエーテル変性シリコーンを併用する方法が開示されているが、耐久透水性や液戻り防止性が不足する。特許文献２ではアルキル燐酸エステル塩に２種類の両性界面活性剤を併用する方法が開示されているが、耐久透水性が不足する。特許文献３ではポリオキシアルキレン脂肪酸アミドのアシル化ポリアミンカチオン化物やアルキルホスフェート塩、両性界面活性剤、ポリオキシアルキレン変性シリコーンを併用する方法が提案されているが、カード通過性や液戻り防止性が不足する。特許文献４ではベタイン型両性活性剤とオキシ脂肪酸エステルのポリアルキレン付加物のジカルボン酸エステルおよびアニオン性界面活性剤を配合した処理剤が開示されているが、カード通過性や瞬時透水性および耐久透水性が不足する。特許文献５ではアルキルホスフェート塩に両性界面活性剤、アルコキシル化リシノレイン型化合物、ポリオキシアルキレン変性シリコーンを併用して繊維を処理する方法が提案されているが、カード通過性や液戻り防止性が不足し、またカードでスカムが発生する。特許文献６ではアルキルホスフェート塩、ポリオキシアルキレン基とアシル基とを有した（ポリ）アミンのカチオン化物、ポリオキシアルキレン基含有ヒドロキシ脂肪酸多価アルコールエステルとジカルボン酸との縮合物の少なくとも１つ以上の水酸基を脂肪酸で封鎖したエステル、ジアルキルスルホサクシネート塩、トリアルキルグリシン誘導体、ポリオキシアルキレン変性シリコーンを併用して繊維を処理する方法が提案されているが、カード通過性や液戻り防止性が不足し、またカードでスカムが発生する。 For example, Patent Document 1 discloses a method in which a polyether-modified silicone is used in combination with an alkyl phosphate ester salt, but it lacks durable water permeability and liquid return prevention properties. Patent Document 2 discloses a method in which two types of amphoteric surfactants are used in combination with an alkyl phosphate ester salt, but the durable water permeability is insufficient. Patent Document 3 proposes a method in which an acylated polyamine cationized product of polyoxyalkylene fatty acid amide, an alkyl phosphate salt, an amphoteric surfactant, and a polyoxyalkylene-modified silicone are used in combination. Run short. Patent Document 4 discloses a treatment agent containing a betaine amphoteric activator, a dicarboxylic acid ester of a polyalkylene adduct of an oxy fatty acid ester, and an anionic surfactant. However, the card passing property, instantaneous water permeability and durable water permeability are disclosed. Lack of sex. Patent Document 5 proposes a method of treating fibers by using an alkyl phosphate salt in combination with an amphoteric surfactant, an alkoxylated ricinolein type compound, and a polyoxyalkylene-modified silicone, but is insufficient in card passage and liquid return prevention properties. In addition, scum is generated on the card. In Patent Document 6, at least one of an alkyl phosphate salt, a cationized product of (poly) amine having a polyoxyalkylene group and an acyl group, and a condensate of a polyoxyalkylene group-containing hydroxy fatty acid polyhydric alcohol ester and a dicarboxylic acid A method has been proposed for treating fibers using a combination of an ester having a hydroxyl group blocked with a fatty acid, a dialkylsulfosuccinate salt, a trialkylglycine derivative, and a polyoxyalkylene-modified silicone. Insufficient and card scum.
このように、これらの処理剤では、現在の衛生材料用途に要求される瞬時透水性、耐久透水性、液戻り防止性には不十分なレベルにあるだけでなく、カチオン性界面活性剤や両性界面活性剤は、皮膚への刺激性が強く、透水性付与剤の不揮発分全体に占めるこれら活性剤の重量割合が例えば１０重量％を超えると、安全性の問題が出てくる。また、ポリオキシアルキレン変性シリコーンを使用することにより液戻り防止性が不十分になったり、不織布の製造工程であるカード機にスカムが発生するという問題が、カード工程の高速化に伴いその頻度が多くなってきている。このように、これらの処理剤では全ての性能レベルを満足することができない。従って、衛生材料用途において、高い性能レベルと安全性を併せ持つ高性能の処理剤が望まれている。 As described above, these treatment agents are not only in an insufficient level for the instantaneous water permeability, durable water permeability, and liquid return prevention required for current hygiene material applications, but also cationic surfactants and amphoteric substances. Surfactants are highly irritating to the skin, and if the weight ratio of these active agents in the entire nonvolatile content of the water-permeability imparting agent exceeds 10% by weight, for example, a safety problem arises. In addition, the use of polyoxyalkylene-modified silicone results in insufficient liquid return prevention, and scum is generated in the card machine, which is a nonwoven fabric manufacturing process. It is getting more. Thus, these treatment agents cannot satisfy all performance levels. Therefore, a high-performance treatment agent having both a high performance level and safety in hygiene material applications is desired.
そこで本発明は、従来の問題点を解決して、瞬時透水性、耐久透水性、液戻り防止性およびカード通過姓のいずれについても高い性能レベルを有し、安全性にも優れた透水性付与剤、それが付着した透水性繊維および不織布を提供するものである。 Therefore, the present invention solves the conventional problems, and has high performance levels in terms of instantaneous water permeability, durable water permeability, liquid return prevention properties and card passing names, and has excellent water permeability. An agent, a water-permeable fiber and a nonwoven fabric to which the agent is attached are provided.
本発明者等は、前記課題を解決するために鋭意検討した結果、透水性能の優れた化合物とポリオレフィンとの親和性が高い化合物を併用することで、その相乗効果により前記課題を解決する透水性付与剤であること、この付与剤を処理して得られる透水性繊維が優れた瞬時透水性、耐久透水性、および液戻り性を有することを見出し、本発明を完成するに至った。 As a result of intensive investigations to solve the above problems, the present inventors have used a compound having excellent water permeability and a compound having high affinity with polyolefin, thereby achieving the water permeability that solves the above problems by its synergistic effect. It was found that the water-permeable fiber obtained by treating the imparting agent was excellent in instantaneous water permeability, durable water permeability, and liquid returnability, and thus completed the present invention.
すなわち、本発明にかかる透水性付与剤は、アルキル基の炭素数が６〜１０である、アルキルホスフェート塩および／またはポリオキシアルキレン基含有アルキルホスフェート塩（Ａ）と、アルキル基の炭素数が１１〜２２である、アルキルホスフェート塩および／またはポリオキシアルキレン基含有アルキルホスフェート塩（Ｂ）と、ポリオキシアルキレン基含有ヒドロキシ脂肪酸多価アルコールエステルとジカルボン酸との縮合物の少なくとも１つ以上の水酸基を脂肪酸で封鎖したエステル（Ｃ）とを必須成分として含む透水性付与剤であって、前記透水性付与剤の不揮発分全体に占める、成分（Ａ）の重量割合が１〜２０重量％、成分（Ｂ）の重量割合が２０〜５０重量％、成分（Ｃ）の重量割合が４１〜６５重量％であり、かつ成分（Ａ）と成分（Ｂ）と成分（Ｃ）の合計の重量割合が８０重量％以上である。 That is, in the water permeability imparting agent according to the present invention, the alkyl phosphate salt and / or polyoxyalkylene group-containing alkyl phosphate salt (A) having an alkyl group having 6 to 10 carbon atoms, and the alkyl group having 11 carbon atoms. An alkyl phosphate salt and / or a polyoxyalkylene group-containing alkyl phosphate salt (B), which is ˜22, and at least one hydroxyl group of a condensate of a polyoxyalkylene group-containing hydroxy fatty acid polyhydric alcohol ester and a dicarboxylic acid; A water-permeability imparting agent comprising, as an essential component, an ester (C) blocked with a fatty acid, wherein the weight percentage of component (A) in the entire nonvolatile content of the water-permeability imparting agent is 1 to 20% by weight, B) is 20 to 50% by weight, component (C) is 41 to 65% by weight, and component The total weight proportion of A) and the component (B) and component (C) is 80 wt% or more.
本発明にかかる透水性付与剤において、前記透水性付与剤の不揮発分全体に占める成分（Ａ）と成分（Ｂ）と成分（Ｃ）の合計の重量割合は、９０重量％以上であることが好ましい。
また、本発明にかかる透水性付与剤は、カチオン性界面活性剤（Ｄ１）、両性界面活性剤（Ｄ２）およびジアルキルスルホサクシネート塩（Ｄ３）から選ばれる少なくとも１種の界面活性剤（Ｄ）をさらに含み、前記透水性付与剤の不揮発分全体に占める界面活性剤（Ｄ）の重量割合が０．２〜１０重量％であることが好ましい。
In the water-permeability imparting agent according to the present invention, the total weight ratio of the component (A), the component (B), and the component (C) in the entire nonvolatile content of the water-permeability imparting agent is 90% by weight or more. preferable.
Further, the water permeability imparting agent according to the present invention is at least one surfactant (D) selected from a cationic surfactant (D1), an amphoteric surfactant (D2) and a dialkylsulfosuccinate salt (D3). It is preferable that the weight ratio of the surfactant (D) in the entire nonvolatile content of the water permeability imparting agent is 0.2 to 10% by weight.
前記成分（Ａ）は下記一般式（１）で示される化合物であることが好ましく、前記成分（Ｂ）は下記一般式（２）で示される化合物であることが好ましい。
前記成分（Ｃ）のポリオキシアルキレン基含有ヒドロキシ脂肪酸多価アルコールエステルは炭素数６〜２２のヒドロキシ脂肪酸と多価アルコールとのエステルのアルキレンオキシド付加物であり、ジカルボン酸の炭素数は２〜１０であり、脂肪酸の炭素数は１０〜５０であることが好ましい。 The polyoxyalkylene group-containing hydroxy fatty acid polyhydric alcohol ester of component (C) is an alkylene oxide adduct of an ester of a hydroxy fatty acid having 6 to 22 carbon atoms and a polyhydric alcohol, and the dicarboxylic acid has 2 to 10 carbon atoms. It is preferable that the fatty acid has 10 to 50 carbon atoms.
前記成分（Ｄ１）は、下記一般式（３）で示される化合物であることが好ましい。
前記成分（Ｄ２）は、下記一般式（４）で示される化合物であることが好ましい。
前記成分（Ｄ３）のアルキル基の炭素数は６〜１８であることが好ましい。 It is preferable that carbon number of the alkyl group of the said component (D3) is 6-18.
また、本発明にかかる透水性付与剤は、不織布製造用ポリオレフィン系繊維に用いられることが好ましい。
本発明の透水性繊維は、不織布製造用ポリオレフィン系繊維に対して、前記の透水性付与剤を処理して得られ、得られた繊維に対する透水性付与剤の不揮発分の付着率が０．１〜２重量％である。
本発明の不織布の製造方法は、前記の透水性繊維を集積させて繊維ウェブを作製し、得られた繊維ウェブを熱処理する工程を含むものである。
Moreover, it is preferable that the water-permeability imparting agent according to the present invention is used for polyolefin fibers for producing nonwoven fabrics.
The water-permeable fiber of the present invention is obtained by treating the polyolefin-based fiber for producing a nonwoven fabric with the above-mentioned water-permeability imparting agent, and the adhesion ratio of the nonvolatile content of the water-permeability imparting agent to the obtained fiber is 0.1. ~ 2% by weight.
The manufacturing method of the nonwoven fabric of this invention includes the process of producing the fiber web by accumulating the said water-permeable fiber, and heat-processing the obtained fiber web.
本発明にかかる透水性付与剤、この透水性付与剤が付着した透水性繊維および不織布は、透水性能の優れた化合物と、ポリオレフィンとの親和性が高い化合物を併用することで、その相乗効果が得られ、その結果、瞬時透水性、耐久透水性、液戻り防止性、カード通過性をも向上させ、さらに安全性にも優れる。 The water-permeability imparting agent according to the present invention, the water-permeable fiber and the nonwoven fabric to which the water-permeability imparting agent is attached, have a synergistic effect by using a compound having excellent water permeability and a compound having high affinity with polyolefin. As a result, instant water permeability, durable water permeability, liquid return prevention property, card passage property are improved, and safety is also excellent.
本発明の透水性付与剤は、アルキル基の炭素数が６〜１０である、アルキルホスフェート塩および／またはポリオキシアルキレン基含有アルキルホスフェート塩（Ａ）と、アルキル基の炭素数が１１〜２２である、アルキルホスフェート塩および／またはポリオキシアルキレン基含有アルキルホスフェート塩（Ｂ）と、ポリオキシアルキレン基含有ヒドロキシ脂肪酸多価アルコールエステルとジカルボン酸との縮合物の少なくとも１つ以上の水酸基を脂肪酸で封鎖したエステル（Ｃ）とを必須成分として含む透水性付与剤であって、前記透水性付与剤の不揮発分全体に占める、成分（Ａ）の重量割合が１〜２０重量％、成分（Ｂ）の重量割合が２０〜５０重量％、成分（Ｃ）の重量割合が４１〜６５重量％であり、かつ成分（Ａ）と成分（Ｂ）と成分（Ｃ）の合計の重量割合が８０重量％以上である。以下、詳細に説明する。 The water permeability imparting agent of the present invention is an alkyl phosphate salt and / or polyoxyalkylene group-containing alkyl phosphate salt (A) having an alkyl group having 6 to 10 carbon atoms, and an alkyl group having 11 to 22 carbon atoms. A certain alkyl phosphate salt and / or polyoxyalkylene group-containing alkyl phosphate salt (B), a polyoxyalkylene group-containing hydroxy fatty acid polyhydric alcohol ester and a condensate of dicarboxylic acid with at least one hydroxyl group blocked with fatty acid The water permeation imparting agent comprising the ester (C) as an essential component, wherein the weight ratio of the component (A) to the whole non-volatile content of the water permeation imparting agent is 1 to 20% by weight of the component (B) The weight ratio is 20 to 50% by weight, the weight ratio of component (C) is 41 to 65% by weight, and component (A) and component (B The total proportion by weight of component (C) is 80 wt% or more. Details will be described below.
〔成分（Ａ）と成分（Ｂ）〕
アルキル基の炭素数が６〜１０である、アルキルホスフェート塩および／またはポリオキシアルキレン基含有アルキルホスフェート塩（Ａ）（成分（Ａ）ということがある）は、本発明の透水性付与剤に必須に含まれる成分である。成分（Ａ）は、瞬時透水性において非常に優れる成分であるが、成分（Ａ）の単独での使用では、カード通過性が劣り耐久透水性を低下させるという欠点がある。
一方、アルキル基の炭素数が１１〜２２である、アルキルホスフェート塩および／またはポリオキシアルキレン基含有アルキルホスフェート塩（Ｂ）（成分（Ｂ）ということがある）も、本発明の透水性付与剤に必須に含まれる成分である。成分（Ｂ）は、カード通過性や耐久透水性を保持する性能および液戻り量を少なくする性能に優れる成分であるが、成分（Ｂ）の単独での使用では、瞬時透水性が劣るという欠点がある。
このように、本発明者等は、アルキルホスフェート塩のアルキル基の炭素数の違いによって瞬時透水性、カード通過性、耐久透水性を保持する性能が異なることを見出し、アルキル基の炭素数が６〜１０の範囲の成分（Ａ）とアルキル基の炭素数が１１〜２２の範囲の成分（Ｂ）を所定量で併用することにより、これらの性能を全て満足させることができることを見出した。
[Component (A) and Component (B)]
The alkyl phosphate salt and / or polyoxyalkylene group-containing alkyl phosphate salt (A) (sometimes referred to as component (A)) having 6 to 10 carbon atoms in the alkyl group is essential for the water permeability imparting agent of the present invention. It is a component contained in. The component (A) is a component that is very excellent in instantaneous water permeability, but the use of the component (A) alone has a drawback that the card permeability is poor and the durable water permeability is lowered.
On the other hand, the alkyl phosphate salt and / or polyoxyalkylene group-containing alkyl phosphate salt (B) (sometimes referred to as component (B)) having 11 to 22 carbon atoms in the alkyl group is also a water permeability imparting agent of the present invention. Is an essential component. Component (B) is a component that is excellent in the performance of maintaining card passage properties and durable water permeability and in reducing the amount of liquid return, but the use of component (B) alone is inferior in instantaneous water permeability. There is.
As described above, the present inventors have found that the performance of maintaining instantaneous water permeability, card permeability, and durable water permeability varies depending on the carbon number of the alkyl group of the alkyl phosphate salt. It was found that by using a component (A) in the range of -10 and component (B) in the range of the carbon number of the alkyl group in the range of 11 to 22 in a predetermined amount, all of these performances can be satisfied.
成分（Ａ）は、アルキル基の炭素数が６〜１０であるアルキルホスフェート塩やアルキル基の炭素数が６〜１０でありポリオキシアルキレン基を含有するアルキルホスフェート塩やこれらの混合物であってもよく、また、１種または２種以上を用いてもよい。
また、成分（Ｂ）は、アルキル基の炭素数が１１〜２２であるアルキルホスフェート塩やアルキル基の炭素数が１１〜２２でありポリオキシアルキレン基を含有するアルキルホスフェート塩やこれらの混合物であってもよく、また、１種または２種以上を用いてもよい。
成分（Ａ）や成分（Ｂ）のアルキル基の炭素数は分布があってもよく、アルキル基は直鎖状であってもよく、分岐を有していてもよい。
Component (A) may be an alkyl phosphate salt having an alkyl group having 6 to 10 carbon atoms, an alkyl phosphate salt having an alkyl group having 6 to 10 carbon atoms and containing a polyoxyalkylene group, or a mixture thereof. Moreover, you may use 1 type (s) or 2 or more types.
Component (B) is an alkyl phosphate salt having an alkyl group having 11 to 22 carbon atoms, an alkyl phosphate salt having an alkyl group having 11 to 22 carbon atoms and containing a polyoxyalkylene group, or a mixture thereof. Moreover, you may use 1 type (s) or 2 or more types.
The carbon number of the alkyl group of component (A) or component (B) may be distributed, and the alkyl group may be linear or branched.
成分（Ａ）は、前述の一般式（１）で示される化合物であることが好ましい。式中、Ｒ１は炭素数６〜１０のアルキル基であり、炭素数は８〜１０が好ましい。アルキル基の炭素数が６未満では、カード工程通過性が低下すると共に製品の臭気が強くなる。
成分（Ｂ）は、前述の一般式（２）で示される化合物であることが好ましい。式中、Ｒ３は炭素数１１〜２２のアルキル基であり、炭素数は１２〜１８が好ましく、１２〜１６がより好ましく、１２〜１４がさらに好ましい。アルキル基の炭素数が２２超であると、化合物の水溶性、カード通過性、瞬時透水性が低下する。
Component (A) is preferably a compound represented by the aforementioned general formula (1). In the formula, R 1 is an alkyl group having 6 to 10 carbon atoms, and preferably 8 to 10 carbon atoms. When the carbon number of the alkyl group is less than 6, the card process passing ability is lowered and the odor of the product is increased.
Component (B) is preferably a compound represented by the aforementioned general formula (2). Wherein, R 3 is an alkyl group having 11 to 22 carbon atoms, the number of carbon atoms preferably 12 to 18, more preferably 12 to 16, 12 to 14 is more preferable. If the alkyl group has more than 22 carbon atoms, the water solubility, card passability, and instantaneous water permeability of the compound will decrease.
成分（Ａ）および成分（Ｂ）において、式中、Ｒ２およびＲ４は、各々独立してエチレン基および／またはプロピレン基である。ｍおよびｐは、各々独立して０〜１５の整数であり、０〜１０が好ましく、０〜８がより好ましく、０〜３がさらに好ましく、０でポリオキシアルキレン基を含有しない場合が特に好ましい。ｎおよびｑは、各々独立して１〜２の整数である。Ｙ１およびＹ２は、各々独立して水素イオン、ナトリウムイオン、カリウムイオン、アンモニウムイオン、ジエタノールアンモニウムイオン、トリエタノールアンモニウムイオンからなる群から選択されるイオン性残基である。 In the component (A) and the component (B), in the formula, R 2 and R 4 are each independently an ethylene group and / or a propylene group. m and p are each independently an integer of 0 to 15, preferably 0 to 10, more preferably 0 to 8, still more preferably 0 to 3, and particularly preferably 0 and no polyoxyalkylene group. . n and q are each independently an integer of 1 to 2. Y 1 and Y 2 are each independently an ionic residue selected from the group consisting of hydrogen ion, sodium ion, potassium ion, ammonium ion, diethanolammonium ion, and triethanolammonium ion.
これらの中でも瞬時透水性の付与という理由から、成分（Ａ）は、オクチルホスフェートカリウム塩、デシルホスフェートカリウム塩、ポリオキシエチレン２モル付加オクチルホスフェートカリウム塩、ポリオキシエチレン３モル付加デシルホスフェートジエタノールアンモニウム塩が好ましく、オクチルホスフェートカリウム塩、デシルホスフェートカリウム塩がさらに好ましい。
一方、成分（Ｂ）は、カード通過性や耐久透水性を保持する性能の向上という理由から、ラウリルホスフェートカリウム塩、ミリスチルホスフェートカリウム塩、セチルホスフェートカリウム塩、ポリオキシエチレン２モル付加セチルホスフェートカリウム塩、ポリオキシエチレン３モル付加ラウリルホスフェートジエタノールアンモニウム塩、ポリオキシエチレン３モル付加ラウリルホスフェートトリエタノールアンモニウム塩が好ましく、ラウリルホスフェートカリウム塩がさらに好ましい。
Among these, the component (A) is composed of octyl phosphate potassium salt, decyl phosphate potassium salt, polyoxyethylene 2 mol addition octyl phosphate potassium salt, polyoxyethylene 3 mol addition decyl phosphate diethanolammonium salt because of providing instant water permeability. Are preferred, and octyl phosphate potassium salt and decyl phosphate potassium salt are more preferred.
On the other hand, the component (B) is composed of lauryl phosphate potassium salt, myristyl phosphate potassium salt, cetyl phosphate potassium salt, polyoxyethylene 2-mole-added cetyl phosphate potassium salt for the purpose of improving the performance of maintaining card permeability and durable water permeability. Polyoxyethylene 3 mol addition lauryl phosphate diethanolammonium salt, polyoxyethylene 3 mol addition lauryl phosphate triethanolammonium salt are preferable, and lauryl phosphate potassium salt is more preferable.
透水性付与剤の不揮発分に占める成分（Ａ）の重量割合は１〜２０重量％であり、２〜１５重量％がより好ましく、２〜１０重量％がさらに好ましい。成分（Ａ）の重量割合が１重量％未満では、瞬時透水性能が低下し、２０重量％超であると、カード通過性が劣り、耐久透水性能を低下させる。
透水性付与剤の不揮発分に占める成分（Ｂ）の重量割合は２０〜５０重量％であり、３０〜５０重量がより好ましく、３５〜４５重量％がさらに好ましく、３７〜４２重量％が特に好ましい。成分（Ｂ）の重量割合が２０重量％未満では、カード通過性を低下させ、５０重量％超であると、瞬時透水性と耐久透水性が低下する。
なお、本発明の透水性付与剤の不揮発分とは、水分などを除くための熱乾燥工程後においても繊維表面に残存する透水性付与剤中の成分を意味し、透水性付与剤を１０５℃で熱処理して水分などを除去し、恒量に達したときの揮発せずに残存した成分を意味する。
The weight ratio of the component (A) in the nonvolatile content of the water permeability imparting agent is 1 to 20% by weight, more preferably 2 to 15% by weight, and further preferably 2 to 10% by weight. When the weight ratio of the component (A) is less than 1% by weight, the instantaneous water permeability is deteriorated, and when it exceeds 20% by weight, the card permeability is inferior and the durable water permeability is deteriorated.
The weight ratio of the component (B) in the nonvolatile content of the water permeability imparting agent is 20 to 50% by weight, more preferably 30 to 50% by weight, further preferably 35 to 45% by weight, and particularly preferably 37 to 42% by weight. . When the weight ratio of the component (B) is less than 20% by weight, the card permeability is lowered, and when it exceeds 50% by weight, the instantaneous water permeability and the durable water permeability are lowered.
The nonvolatile content of the water-permeability imparting agent of the present invention means a component in the water-permeability imparting agent remaining on the fiber surface even after the heat drying step for removing moisture and the like. It means a component that remains without being volatilized when it reaches a constant weight by removing heat and the like by heat treatment.
〔成分（Ｃ）〕
ポリオキシアルキレン基含有ヒドロキシ脂肪酸多価アルコールエステル（以下、ポリヒドロキシエステルということがある）とジカルボン酸との縮合物の少なくとも１つの水酸基を脂肪酸で封鎖したエステル（Ｃ）（成分（Ｃ）ということがある）は、本発明の透水性付与剤に必須に含まれる成分であり、ポリオレフィンとの親和性が高いので、繊維に付着した付与剤は水と接触しても繊維から脱落し難くなる。その結果、繰り返し透水性を維持できる成分である。
[Component (C)]
Polyoxyalkylene group-containing hydroxy fatty acid polyhydric alcohol ester (hereinafter sometimes referred to as polyhydroxy ester) and a condensate of dicarboxylic acid with at least one hydroxyl group blocked with fatty acid ester (C) (component (C) Is a component that is essentially included in the water-permeability imparting agent of the present invention, and has high affinity with polyolefin, so that the imparting agent attached to the fiber is difficult to come off from the fiber even when it comes into contact with water. As a result, it is a component that can maintain water permeability repeatedly.
ポリヒドロキシエステルは、構造上、ポリオキシアルキレン基含有ヒドロキシ脂肪酸と多価アルコールとのエステルであり、多価アルコールの水酸基のうち、２個以上（好ましくは全部）の水酸基がエステル化されている。したがって、ポリオキシアルキレン基含有ヒドロキシ脂肪酸多価アルコールエステルは、複数の水酸基を有するエステルである。 The polyhydroxyester is structurally an ester of a polyoxyalkylene group-containing hydroxy fatty acid and a polyhydric alcohol, and two or more (preferably all) hydroxyl groups of the polyhydric alcohol are esterified. Therefore, the polyoxyalkylene group-containing hydroxy fatty acid polyhydric alcohol ester is an ester having a plurality of hydroxyl groups.
ポリオキシアルキレン基含有ヒドロキシ脂肪酸は、脂肪酸の炭化水素基に酸素原子を介してポリオキシアルキレン基が結合した構造を有し、ポリオキシアルキレン基の脂肪酸の炭化水素基と結合していない片末端が水酸基となっている。
ポリヒドロキシエステルとしては、たとえば、炭素数６〜２２（好ましくは１２〜２２）のヒドロキシ脂肪酸と多価アルコールとのエステル化物のアルキレンオキシド付加物を挙げることができる。ヒドロキシ脂肪酸の炭素数が６未満であると、親水性が強くなり、一方、２２を超えると疎水性が強くなる。いずれの場合も他の成分との相溶性が悪くなるため、十分な耐久透水性を得られないことがある。
The polyoxyalkylene group-containing hydroxy fatty acid has a structure in which a polyoxyalkylene group is bonded to a fatty acid hydrocarbon group via an oxygen atom, and one end that is not bonded to the fatty acid hydrocarbon group of the polyoxyalkylene group is It is a hydroxyl group.
Examples of the polyhydroxyester include an alkylene oxide adduct of an esterified product of a hydroxy fatty acid having 6 to 22 carbon atoms (preferably 12 to 22 carbon atoms) and a polyhydric alcohol. When the number of carbon atoms of the hydroxy fatty acid is less than 6, the hydrophilicity becomes strong, while when it exceeds 22, the hydrophobicity becomes strong. In either case, the compatibility with other components deteriorates, so that sufficient durable water permeability may not be obtained.
炭素数６〜２２のヒドロキシ脂肪酸としては、たとえば、ヒドロキシカプリル酸、ヒドロキシカプリン酸、ヒドロキシウンデカン酸、ヒドロキシラウリン酸、ヒドロキシステアリン酸、リシノール酸挙げられ、ヒドロキシステアリン酸、リシノール酸が好ましい。多価アルコールとしては、たとえば、エチレングリコール、グリセリン、ソルビタン、トリメチロールプロパン、ペンタエリスリトール等が挙げられ、グリセリンが好ましい。アルキレンオキシドとしては、エチレンオキシド、プロピレンオキシド、ブチレンオキシド等の炭素数２〜４のアルキレンオキシドが挙げられる。 Examples of the hydroxy fatty acid having 6 to 22 carbon atoms include hydroxycaprylic acid, hydroxycapric acid, hydroxyundecanoic acid, hydroxylauric acid, hydroxystearic acid, and ricinoleic acid, and hydroxystearic acid and ricinoleic acid are preferable. Examples of the polyhydric alcohol include ethylene glycol, glycerin, sorbitan, trimethylolpropane, pentaerythritol and the like, and glycerin is preferable. Examples of the alkylene oxide include C2-C4 alkylene oxides such as ethylene oxide, propylene oxide, and butylene oxide.
アルキレンオキシドの付加モル数は、上記ヒドロキシ脂肪酸多価アルコールエステルの水酸基１モル当量当り、好ましくは８０以下、さらに好ましくは５〜３０である。付加モル数が８０を超えると液戻り量が増加することがあるので好ましくない。高い耐久透水性を得るためには、親水基と疎水基のバランスを調整することが重要である。アルキレンオキシドに占めるエチレンオキシドの割合は、好ましくは５０モル％以上、さらに好ましくは８０モル％以上である。エチレンオキシドの割合が５０モル％未満では、疎水性が強くなるために十分な耐久透水性が得られないことがある。 The number of moles of alkylene oxide added is preferably 80 or less, more preferably 5-30, per mole equivalent of hydroxyl group of the hydroxy fatty acid polyhydric alcohol ester. If the added mole number exceeds 80, the liquid return amount may increase, which is not preferable. In order to obtain high durable water permeability, it is important to adjust the balance between the hydrophilic group and the hydrophobic group. The proportion of ethylene oxide in the alkylene oxide is preferably 50 mol% or more, more preferably 80 mol% or more. If the ratio of ethylene oxide is less than 50 mol%, the hydrophobicity becomes strong and sufficient durable water permeability may not be obtained.
ポリヒドロキシエステルは、たとえば、多価アルコールとヒドロキシ脂肪酸（ヒドロキシモノカルボン酸）を通常の条件でエステル化してエステル化物を得て、次いでこのエステル化物にアルキレンオキシドを付加反応させることによって製造できる。ポリヒドロキシエステルは、ひまし油などの天然から得られる油脂やこれに水素を添加した硬化ひまし油を用い、さらにアルキレンオキシドを付加反応させることによっても、好適に製造できる。
ポリヒドロキシエステルを製造する場合、多価アルコールの水酸基１モル当量あたりのヒドロキシ脂肪酸のカルボキシル基モル当量は、０．５〜１の範囲であることが好ましい。
The polyhydroxyester can be produced, for example, by esterifying a polyhydric alcohol and a hydroxy fatty acid (hydroxymonocarboxylic acid) under ordinary conditions to obtain an esterified product, and then subjecting the esterified product to an addition reaction with an alkylene oxide. The polyhydroxyester can be suitably produced also by using an oil and fat obtained from nature such as castor oil or a hardened castor oil obtained by adding hydrogen to this, and further subjecting it to an addition reaction with an alkylene oxide.
When manufacturing a polyhydroxyester, it is preferable that the carboxyl group molar equivalent of the hydroxy fatty acid per 1 molar equivalent of the hydroxyl group of a polyhydric alcohol is the range of 0.5-1.
ポリヒドロキシエステルとジカルボン酸との縮合物において、ジカルボン酸の炭素数は、２〜１０が好ましく、２〜８がさらに好ましい。ジカルボン酸の炭素数が１０を超えると十分な親水性を付与できないことがある。このようなジカルボン酸としては、たとえば、シュウ酸、マロン酸、コハク酸、グルタル酸、アジピン酸、ピメリン酸、スベリン酸、アゼライン酸、セバシン酸、マレイン酸、フタル酸等が挙げられる。ジカルボン酸と共に、ラウリン酸、オレイン酸、ステアリン酸、ベヘン酸、安息香酸等のジカルボン酸以外のカルボン酸を２０％以下（好ましくは１０％以下）含有しても良い。ポリヒドロキシエステルとジカルボン酸との縮合物を製造する場合、ポリヒドロキシエステルの水酸基1モル当量あたりのジカルボン酸のカルボキシル基モル当量は、０．２〜１の範囲であることが好ましく、０．４〜０．８がさらに好ましい。エステル化の反応は通常の条件で良く、特に限定はない。 In the condensate of a polyhydroxyester and a dicarboxylic acid, the carbon number of the dicarboxylic acid is preferably 2 to 10, and more preferably 2 to 8. If the carbon number of the dicarboxylic acid exceeds 10, sufficient hydrophilicity may not be imparted. Examples of such dicarboxylic acids include oxalic acid, malonic acid, succinic acid, glutaric acid, adipic acid, pimelic acid, suberic acid, azelaic acid, sebacic acid, maleic acid, and phthalic acid. Along with the dicarboxylic acid, a carboxylic acid other than the dicarboxylic acid such as lauric acid, oleic acid, stearic acid, behenic acid and benzoic acid may be contained in an amount of 20% or less (preferably 10% or less). When producing the condensate of polyhydroxyester and dicarboxylic acid, the carboxyl group molar equivalent of dicarboxylic acid per molar equivalent of hydroxyl group of polyhydroxyester is preferably in the range of 0.2 to 1, -0.8 is more preferable. The esterification reaction may be performed under ordinary conditions and is not particularly limited.
本発明の成分（Ｃ）は、上述のポリオキシアルキレン基含有ヒドロキシ脂肪酸多価アルコールエステルとジカルボン酸との縮合物（以下、縮合物ということがある）において、少なくとも１つの水酸基を脂肪酸で封鎖したエステルである。特許文献４のような脂肪酸で封鎖していないエステルでは、耐久透水性能が不足し、また化合物が経時的に増粘し水不溶物が増加するので、付与剤の溶液安定性が低下する。
縮合物の少なくとも１つ以上の水酸基を封鎖する脂肪酸の炭素数について、１０〜２２の範囲だけでなく、１０〜５０の範囲においても使用することが可能である。すなわち、封鎖する脂肪酸の炭素数は１０〜５０が好ましく、１２〜３６がさらに好ましい。また、脂肪酸の炭素数が１０未満であると親水性が強くなり、一方、５０を超えると疎水性が強くなる。このように、親水性と疎水性とがアンバランスであると、十分な耐久透水性を得ることができないことがある。このような脂肪酸としては、たとえば、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、イコサン酸、ベヘン酸、リグノセリン酸、ネルボン酸、セロチン酸、モンタン酸、メリシン酸、ラノリン脂肪酸等が挙げられるが、ベヘン酸やウールグリースを精製したラノリン誘導体である炭素数１２〜３６のラノリン脂肪酸が好ましい。縮合物と脂肪酸とのエステルを製造する場合、縮合物の水酸基1モル当量あたりの脂肪酸のカルボキシル基モル当量は０．２〜１の範囲であることが好ましく、０．４〜１がさらに好ましい。エステル化の反応条件については特に限定はない。
Component (C) of the present invention is a condensate (hereinafter sometimes referred to as a condensate) of a polyoxyalkylene group-containing hydroxy fatty acid polyhydric alcohol ester and a dicarboxylic acid, wherein at least one hydroxyl group is blocked with a fatty acid. Ester. An ester not blocked with a fatty acid as in Patent Document 4 has insufficient durable water permeability, and the compound thickens over time and water insoluble matter increases, so that the solution stability of the imparting agent decreases.
The carbon number of the fatty acid blocking at least one hydroxyl group of the condensate can be used not only in the range of 10 to 22 but also in the range of 10 to 50. That is, the number of carbon atoms of the fatty acid to be blocked is preferably 10 to 50, and more preferably 12 to 36. Further, when the number of carbon atoms of the fatty acid is less than 10, the hydrophilicity becomes strong, and when it exceeds 50, the hydrophobicity becomes strong. Thus, when hydrophilicity and hydrophobicity are unbalanced, sufficient durable water permeability may not be obtained. Examples of such fatty acids include lauric acid, myristic acid, palmitic acid, stearic acid, oleic acid, icosanoic acid, behenic acid, lignoceric acid, nervonic acid, serotic acid, montanic acid, melicic acid, lanolin fatty acid and the like. However, lanolin fatty acid having 12 to 36 carbon atoms, which is a lanolin derivative obtained by purifying behenic acid or wool grease, is preferred. When the ester of the condensate and the fatty acid is produced, the carboxyl group molar equivalent of the fatty acid per 1 molar equivalent of the hydroxyl group of the condensate is preferably in the range of 0.2 to 1, and more preferably 0.4 to 1. There are no particular limitations on the reaction conditions for esterification.
透水性付与剤の不揮発分に占める成分（Ｃ）の重量割合は４１〜６５重量％であり、４３〜６５重量％がより好ましく、４５〜６５重量％がさらに好ましく、５０〜６５重量％が特に好ましい。成分（Ｃ）の重量割合が４１重量％未満では、瞬時透水性は向上するが耐久透水性が低下する。一方、成分（Ｃ）の重量割合が６５重量％超であると、耐久透水性は向上するがカード通過性が低下する。 The weight ratio of the component (C) in the nonvolatile content of the water permeability imparting agent is 41 to 65% by weight, more preferably 43 to 65% by weight, still more preferably 45 to 65% by weight, and particularly preferably 50 to 65% by weight. preferable. When the weight ratio of the component (C) is less than 41% by weight, the instantaneous water permeability is improved, but the durable water permeability is lowered. On the other hand, when the weight ratio of the component (C) is more than 65% by weight, the durable water permeability is improved, but the card passing property is lowered.
このように、瞬時透水性能に優れた成分（Ａ）と、カード通過性能、耐久透水性を保持する性能、液戻り量を少なくする性能に優れた成分（Ｂ）に、さらにポリオレフィンとの親和性が高い成分（Ｃ）を所定量併用することで、その相乗効果により、瞬時透水性、耐久透水性、カード通過性等を向上することができる。さらに、カチオン性界面活性剤や両性界面活性剤、ジアルキルスルホサクシネート塩等を最小限に留めることができ、安全性に優れる。これらの効果をより発揮させるために、透水性付与剤の不揮発分に占める成分（Ａ）と成分（Ｂ）と成分（Ｃ）の合計の重量割合は８０重量％以上であり、好ましくは９０重量％以上、さらに好ましくは９５重量％以上である。重量割合が８０重量％未満では、細胞毒性が悪化するとともにカード機でシリンダー巻付きが多くなり均一なウェブが得られなくなる。 As described above, the component (A) excellent in instantaneous water permeation performance, the card passage performance, the performance of maintaining durable water permeability, and the component (B) excellent in performance of reducing the liquid return amount are further compatible with polyolefin. In combination with a predetermined amount of the component (C) having a high value, instantaneous water permeability, durable water permeability, card permeability and the like can be improved by the synergistic effect. Furthermore, cationic surfactants, amphoteric surfactants, dialkylsulfosuccinate salts and the like can be kept to a minimum, and the safety is excellent. In order to exhibit these effects more, the total weight ratio of the component (A), the component (B), and the component (C) in the nonvolatile content of the water permeability imparting agent is 80% by weight or more, preferably 90% by weight. % Or more, more preferably 95% by weight or more. When the weight ratio is less than 80% by weight, the cytotoxicity is deteriorated and the winding of the cylinder is increased in the card machine, so that a uniform web cannot be obtained.
〔界面活性剤（Ｄ）〕
本発明の透水性付与剤は、耐久透水性を補助する成分として、カチオン性界面活性剤（Ｄ１）、両性界面活性剤（Ｄ２）およびジアルキルスルホサクシネート塩（Ｄ３）から選ばれる少なくとも１種の界面活性剤（Ｄ）を、安全性を損なわない範囲で含んでもよい。透水性付与剤の不揮発分全体に占める界面活性剤（Ｄ）の重量割合は０．２〜１０重量％が好ましく、１〜７重量％がより好ましく、２〜５重量％がさらに好ましく、２〜４重量％が特に好ましい。重量割合が１０重量％超になると、皮膚刺激性が高くなる懸念があり、細胞毒性が悪化することがある。
[Surfactant (D)]
The water-permeability imparting agent of the present invention is at least one selected from a cationic surfactant (D1), an amphoteric surfactant (D2) and a dialkylsulfosuccinate salt (D3) as a component for assisting durable water permeability. Surfactant (D) may be included as long as safety is not impaired. The weight ratio of the surfactant (D) in the entire nonvolatile content of the water permeability imparting agent is preferably 0.2 to 10% by weight, more preferably 1 to 7% by weight, further preferably 2 to 5% by weight, 4% by weight is particularly preferred. When the weight ratio exceeds 10% by weight, there is a concern that the skin irritation becomes high, and the cytotoxicity may be deteriorated.
前記のカチオン性界面活性剤（Ｄ１）（成分（Ｄ１）ということがある）は、前述の一般式（３）で示される化合物であることが好ましい。式中、Ｒ５は炭素数８〜２４の脂肪族炭化水素基であり、Ｒ６はＲ５が炭素数８〜１８の肪族炭化水素基のときには、炭素数８〜１８の脂肪族炭化水素基であり、Ｒ５が炭素数１９〜２４の脂肪族炭化水素基のときには、水素原子、炭素数１〜３の脂肪族炭化水素基または炭素数１〜３のヒドロキシアルキル基である。Ｒ７およびＲ８は各々独立して水素原子、炭素数１〜３の脂肪族炭化水素基または炭素数１〜３のヒドロキシアルキル基である。Ｘはハロゲンイオン、硝酸イオン、酢酸イオン、メチル硫酸イオン、エチル硫酸イオンおよびジメチル燐酸イオンからなる群から選択されるイオン性残基である。Ｒ５、Ｒ６、Ｒ７およびＲ８の脂肪族炭化水素基は、飽和であっても不飽和であってもよく、また直鎖状であってもよく、分岐を有していてもよい。成分（Ｄ１）は、単独または２種以上併用することができる。 The cationic surfactant (D1) (sometimes referred to as component (D1)) is preferably a compound represented by the general formula (3). In the formula, R 5 is an aliphatic hydrocarbon group having 8 to 24 carbon atoms, and R 6 is an aliphatic hydrocarbon group having 8 to 18 carbon atoms when R 5 is an aliphatic hydrocarbon group having 8 to 18 carbon atoms. And when R 5 is an aliphatic hydrocarbon group having 19 to 24 carbon atoms, it is a hydrogen atom, an aliphatic hydrocarbon group having 1 to 3 carbon atoms, or a hydroxyalkyl group having 1 to 3 carbon atoms. R 7 and R 8 are each independently a hydrogen atom, an aliphatic hydrocarbon group having 1 to 3 carbon atoms, or a hydroxyalkyl group having 1 to 3 carbon atoms. X is an ionic residue selected from the group consisting of halogen ions, nitrate ions, acetate ions, methyl sulfate ions, ethyl sulfate ions and dimethyl phosphate ions. The aliphatic hydrocarbon groups for R 5 , R 6 , R 7 and R 8 may be saturated or unsaturated, may be linear, and may have a branch. . Component (D1) can be used alone or in combination of two or more.
Ｒ５の炭素数が８未満の場合は、カード通過性が悪化するとともに、親水性が強くなり過ぎて耐久透水性が低下し、液戻り性が増加し易くなることがある。Ｒ５の炭素数が２４超の場合は、瞬時透水性が低下し易くなることがある。Ｒ７とＲ８は、好ましくは炭素数１〜３の脂肪族炭化水素基である。Ｒ７とＲ８のいずれかの炭素数が３超では、瞬時透水性および耐久透水性が低下し易くなることがある。 When the carbon number of R 5 is less than 8, the card passing property is deteriorated, the hydrophilicity becomes too strong, the durable water permeability is lowered, and the liquid return property is likely to increase. If the carbon number of R 5 is 24 greater than is the instantaneous water permeability tends to decrease. R 7 and R 8 are preferably an aliphatic hydrocarbon group having 1 to 3 carbon atoms. If any one of R 7 and R 8 has more than 3 carbon atoms, instantaneous water permeability and durable water permeability may be likely to be lowered.
一般式（３）で表されるカチオン性界面活性剤の例としては、ジオクチルジメチルアンモニウムクロライド、ジデシルジメチルアンモニウムクロライド、ジラウリルジメチルアンモニウムクロライド、ジステアリルジメチルアンモニウムクロライド、ジ椰子アルキルジメチルアンモニウムクロライド、ジ硬化牛脂アルキルジメチルアンモニウムクロライド、ベヘニルトリメチルアンモニウムクロライド、ジラウリルジメチルアンモニウムメトサルフェート、ジラウリルメチルエチルアンモニウムエトサルフェート等が挙げられ、これらの中でも、ジステアリルジメチルアンモニウムクロライドやベヘニルトリメチルアンモニウムクロライドが好ましい。 Examples of the cationic surfactant represented by the general formula (3) include dioctyldimethylammonium chloride, didecyldimethylammonium chloride, dilauryldimethylammonium chloride, distearyldimethylammonium chloride, dicoco alkyldimethylammonium chloride, di Cured beef tallow alkyldimethylammonium chloride, behenyltrimethylammonium chloride, dilauryldimethylammonium methosulfate, dilaurylmethylethylammonium etosulphate and the like can be mentioned. Among these, distearyldimethylammonium chloride and behenyltrimethylammonium chloride are preferable.
〔成分（Ｄ２）〕
前記の両性界面活性剤（Ｄ２）（成分（Ｄ２）ということがある）としては、トリアルキルグリシン型両性界面活性剤、アルキルアミドプロピルグリシン型両性界面活性剤等が挙げられ、一般式（４）で表される両性界面活性剤であることが好ましい。式中、ａは１〜３の整数であり、ｂは０または１であり、Ｒ９は炭素数６〜２２の炭化水素基であり、Ｒ１０およびＲ１１は各々独立して炭素数１〜３の炭化水素基である。Ｒ９、Ｒ１０およびＲ１１の炭化水素基は、脂肪族炭化水素基が好ましく、飽和であっても不飽和であってもよく、また直鎖状であってもよく、分岐を有していてもよい。成分（Ｄ２）は、単独または２種以上併用することができる。
[Component (D2)]
Examples of the amphoteric surfactant (D2) (sometimes referred to as component (D2)) include trialkyl glycine-type amphoteric surfactants, alkylamidopropyl glycine-type amphoteric surfactants, and the general formula (4) It is preferable that it is an amphoteric surfactant represented by these. In the formula, a is an integer of 1 to 3, b is 0 or 1, R 9 is a hydrocarbon group having 6 to 22 carbon atoms, and R 10 and R 11 are each independently 1 to 1 carbon atom. 3 hydrocarbon groups. The hydrocarbon group for R 9 , R 10 and R 11 is preferably an aliphatic hydrocarbon group, which may be saturated or unsaturated, may be linear, and has a branch. May be. Component (D2) can be used alone or in combination of two or more.
一般式（４）で表されるトリアルキルグリシン型両性界面活性剤は、式中、ｂは０であり、Ｒ９は炭素数６〜２２の炭化水素基であり、炭素数は１６〜２２が好ましい。炭素数が６未満の場合は、親水性が強くなり過ぎて耐久透水性が低下し、液戻り性が増加し易くなることがある。一方、炭素数が２２超の場合は、瞬時透水性が低下し易くなることがある。Ｒ１０およびＲ１１は、いずれも炭素数１〜３の炭化水素基である。一例としては、ジメチルドデシルグリシンヒドロキサイド、ジメチルテトラデシルグリシンヒドロキサイド、ジメチルヘキサデシルグリシンヒドロキサイド、ジメチルオクタデシルグリシンヒドロキサイド等を挙げることができる。
一方、一般式（４）で表されるアルキルアミドプロピルグリシン型両性界面活性剤は、式中、ｂは１であり、ａは１〜３の整数であり、Ｒ９は炭素数６〜２２の炭化水素基であり、炭素数は１１〜２２が好ましい。炭素数が６未満の場合は、親水性が強くなり過ぎて耐久透水性が低下し、液戻り性が増加し易くなることがある。一方、炭素数が２２超の場合は、瞬時透水性が低下し易くなることがある。Ｒ１０およびＲ１１は、いずれも炭素数１〜３の炭化水素基である。一例としては、ヤシ油脂肪酸アミドプロピルベタイン、ラウリン酸アミドプロピルベタイン、ステアリン酸アミドエチルベタイン等を挙げることができる。
In the trialkylglycine type amphoteric surfactant represented by the general formula (4), b is 0, R 9 is a hydrocarbon group having 6 to 22 carbon atoms, and the carbon number is 16 to 22 preferable. When the number of carbon atoms is less than 6, the hydrophilicity becomes too strong, the durable water permeability may be lowered, and the liquid return property may be easily increased. On the other hand, when the number of carbon atoms exceeds 22, the instantaneous water permeability may be easily lowered. R 10 and R 11 are both hydrocarbon groups having 1 to 3 carbon atoms. Examples include dimethyl dodecyl glycine hydroxide, dimethyl tetradecyl glycine hydroxide, dimethyl hexadecyl glycine hydroxide, dimethyl octadecyl glycine hydroxide, and the like.
On the other hand, the alkylamidopropylglycine-type amphoteric surfactant represented by the general formula (4) has a formula in which b is 1, a is an integer of 1 to 3, and R 9 has 6 to 22 carbon atoms. A hydrocarbon group, preferably having 11 to 22 carbon atoms. When the number of carbon atoms is less than 6, the hydrophilicity becomes too strong, the durable water permeability may be lowered, and the liquid return property may be easily increased. On the other hand, when the number of carbon atoms exceeds 22, the instantaneous water permeability may be easily lowered. R 10 and R 11 are both hydrocarbon groups having 1 to 3 carbon atoms. Examples include coconut oil fatty acid amidopropyl betaine, lauric acid amidopropyl betaine, and stearic acid amidoethyl betaine.
〔成分（Ｄ３）〕
前記のジアルキルスルホサクシネート塩（Ｄ３）（成分（Ｄ３）ということがある）は、α位にスルホン酸塩の基を有するコハク酸のジアルキルエステルである。ジアルキルエステルを構成するアルキル基の炭素数は６〜１８が好ましく、８〜１８がより好ましく、１０〜１８がさらに好ましく、１２〜１４が特に好ましい。アルキル基の炭素数が６未満ではカード通過性が低下することがある。一方、アルキル基の炭素数が１８超であると、瞬時透水性が低下することがある。
[Component (D3)]
The dialkyl sulfosuccinate salt (D3) (sometimes referred to as component (D3)) is a dialkyl ester of succinic acid having a sulfonate group at the α-position. 6-18 are preferable, as for carbon number of the alkyl group which comprises dialkyl ester, 8-18 are more preferable, 10-18 are more preferable, and 12-14 are especially preferable. If the alkyl group has less than 6 carbon atoms, the card passing property may decrease. On the other hand, if the carbon number of the alkyl group exceeds 18, the instantaneous water permeability may decrease.
成分（Ｄ３）のスルホン酸塩としては、ナトリウム塩やカリウム塩等のアルカリ金属塩、アミン塩を挙げることができ、ナトリウム塩および／またはカリウム塩であると、透水性付与剤が付着した繊維に液体が速やかに浸透するので好ましい。 Examples of the sulfonate salt of component (D3) include alkali metal salts such as sodium salt and potassium salt, and amine salts. When the salt is sodium salt and / or potassium salt, the fiber to which the water permeability-imparting agent has adhered is attached. This is preferable because the liquid penetrates quickly.
〔その他の成分〕
本発明の透水性付与剤は、本発明の効果を阻害しない範囲でポリオキシアルキレン変性シリコーン（Ｅ）（成分（Ｅ）ということがある）を含有してもよいが、液戻り防止性が不足するという問題とカード時にスカムが発生するという理由から、実質的に含有しないことが好ましく、具体的には、透水性付与剤の不揮発分全体に占めるシリコーン系化合物（Ｅ）の重量割合は１重量％未満が好ましい。成分（Ｅ）は、分子量が１，０００〜１００，０００であり、Ｓｉ含有率が２０〜７０重量％である。ポリオキシアルキレンはポリオキシエチレンやポリオキシプロピレンであり、ポリオキシアルキレン全体のうちポリオキシエチレンが占める割合が２０重量％以上である。
[Other ingredients]
The water permeability-imparting agent of the present invention may contain polyoxyalkylene-modified silicone (E) (sometimes referred to as component (E)) as long as it does not impair the effects of the present invention, but lacks liquid return prevention properties. In view of the problem of scum and the fact that scum is generated at the time of carding, it is preferably not substantially contained. Specifically, the weight ratio of the silicone compound (E) in the entire nonvolatile content of the water permeability imparting agent is 1 weight. % Is preferred. Component (E) has a molecular weight of 1,000 to 100,000 and a Si content of 20 to 70% by weight. Polyoxyalkylene is polyoxyethylene or polyoxypropylene, and the proportion of polyoxyethylene in the whole polyoxyalkylene is 20% by weight or more.
本発明の透水性付与剤は、必要に応じて水および／または溶剤を含有していてもよく、水を必須に含有することが好ましい。本発明に使用する水としては、純水、蒸留水、精製水、軟水、イオン交換水、水道水等のいずれであってもよい。透水性付与剤を製造する際の透水性付与剤全体に占める不揮発分の重量割合は、１０〜２５重量％が好ましく、１８〜２３重量％が特に好ましい。
また、本発明の透水性付与剤は、皮膚への刺激性の面から、透水性付与剤全体に占める不揮発分の重量割合を１重量％としたときの水性液のｐＨ（２０℃）が５〜８の範囲になることが好ましい。
The water-permeability imparting agent of the present invention may contain water and / or a solvent as necessary, and preferably contains water essentially. The water used in the present invention may be any of pure water, distilled water, purified water, soft water, ion exchange water, tap water and the like. 10 to 25 weight% is preferable and, as for the weight ratio of the non volatile matter to the whole water-permeability imparting agent at the time of manufacturing a water-permeability imparting agent, 18 to 23 weight% is especially preferable.
In addition, the water-permeability imparting agent of the present invention has an aqueous liquid pH (20 ° C.) of 5% when the weight ratio of the non-volatile content in the entire water-permeability imparting agent is 1% by weight from the viewpoint of irritation to the skin. It is preferable to be in the range of ˜8.
また、本発明の透水性付与剤には、必要に応じて、抗菌剤、酸化防止剤、防腐剤、艶消し剤、顔料、抗菌剤、芳香剤、消泡剤等がさらに含まれていてもよい。 The water permeability imparting agent of the present invention may further contain an antibacterial agent, an antioxidant, a preservative, a matting agent, a pigment, an antibacterial agent, a fragrance, an antifoaming agent, etc. Good.
〔透水性付与剤の製造方法〕
本発明の透水性付与剤の製造方法としては、特に限定されず、公知の方法を採用できる。例えば、成分（Ａ）の水溶液に、成分（Ｂ）の水溶液を配合し約７０℃の温度で撹伴する。撹伴を続けながら通常のエステル反応で合成したポリオキシアルキレン基含有ヒドロキシ脂肪酸多価アルコールエステルとジカルボン酸との縮合物の少なくとも１つの水酸基を脂肪酸で封鎖したエステル（Ｃ）を加え同温度で均一に撹伴する。次に、必要に応じて成分（Ｄ１）、成分（Ｄ２）および成分（Ｄ３）から選ばれる少なくとも１種の界面活性剤（Ｄ）の水溶液を配合して約５０℃の温度で均一に攪拌する。次いで、攪拌しながら所定量の水を注入し希釈すると２０重量％の透水性付与剤が得ることができる。
[Method for producing water permeability imparting agent]
It does not specifically limit as a manufacturing method of the water-permeability imparting agent of this invention, A well-known method is employable. For example, the aqueous solution of component (B) is blended with the aqueous solution of component (A) and stirred at a temperature of about 70 ° C. Uniform at the same temperature by adding an ester (C) in which at least one hydroxyl group of a polyoxyalkylene group-containing hydroxy fatty acid polyhydric alcohol ester and dicarboxylic acid synthesized by a normal ester reaction is blocked with a fatty acid while stirring is continued. Stir to. Next, if necessary, an aqueous solution of at least one surfactant (D) selected from component (D1), component (D2) and component (D3) is blended and stirred uniformly at a temperature of about 50 ° C. . Next, when a predetermined amount of water is poured and diluted while stirring, a water-permeability imparting agent of 20% by weight can be obtained.
〔透水性繊維〕
本発明の透水性繊維は、繊維本体とこれに付着した上記透水性付与剤とから構成される透水性繊維であり、一般的には所定の長さに切断した短繊維である。透水性付与剤の付着率は、前記透水性繊維に対して０．１〜２重量％であり、好ましくは０．３〜１重量％である。透水性繊維に対する透水性付与剤の付着率が０．１重量％未満では、瞬時透水性、耐久透水性が低下することがある。一方、透水性付与剤の付着率が２重量％を超えると、繊維をカード処理する時に巻付きが多くなって生産性が大幅に低下し、乾式法等の方法により得られた不織布等の繊維製品が透水後にベトツキが大きくなることがある。
[Water-permeable fiber]
The water-permeable fiber of the present invention is a water-permeable fiber composed of a fiber main body and the water-permeability imparting agent attached thereto, and is generally a short fiber cut to a predetermined length. The adhesion rate of the water-permeability imparting agent is 0.1 to 2% by weight, preferably 0.3 to 1% by weight, based on the water-permeable fiber. When the adhesion rate of the water permeability imparting agent to the water permeable fiber is less than 0.1% by weight, the instantaneous water permeability and the durable water permeability may be lowered. On the other hand, when the adhesion rate of the water permeability-imparting agent exceeds 2% by weight, the amount of wrapping is increased when the fiber is carded, resulting in a significant reduction in productivity, and fibers such as nonwoven fabric obtained by a method such as a dry method. The product may become sticky after water permeation.
繊維本体としては、たとえば、ポリオレフィン繊維、ポリエステル繊維、ナイロン繊維、塩ビ繊維、２種類以上の熱可塑性樹脂からなる複合繊維等であり、複合繊維の組み合わせとしては、ポリオレフィン系樹脂／ポリオレフィン系樹脂の場合、例えば、高密度ポリエチレン／ポリプロピレン、直鎖状高密度ポリエチレン／ポリプロピレン、低密度ポリエチレン／ポリプロピレン、プロピレンと他のα−オレフィンとの二元共重合体または三元共重合体／ポリプロピレン、直鎖状高密度ポリエチレン／高密度ポリエチレン、低密度ポリエチレン／高密度ポリエチレン等が挙げられる。また、ポリオレフィン系樹脂／ポリエステル系樹脂の場合、例えば、ポリプロピレン／ポリエチレンテレフタレート、高密度ポリエチレン／ポリエチレンテレフタレート、直鎖状高密度ポリエチレン／ポリエチレンテレフタレート、低密度ポリエチレン／ポリエチレンテレフタレート等が挙げられる。また、ポリエステル系樹脂／ポリエステル系樹脂の場合、例えば、共重合ポリエステル／ポリエチレンテレフタレート等が挙げられる。さらにポリアミド系樹脂／ポリエステル系樹脂、ポリオレフィン系樹脂／ポリアミド系樹脂等からなる繊維も例示することができる。これら繊維のなかでも、付着した透水性付与剤が尿や体液等の液体によって脱落がし難いという理由から、不織布製造用ポリオレフィン系繊維に本発明の透水性付与剤は好適である。 Examples of the fiber body include polyolefin fibers, polyester fibers, nylon fibers, polyvinyl chloride fibers, composite fibers composed of two or more types of thermoplastic resins, and the combination of the composite fibers is a polyolefin resin / polyolefin resin. , For example, high density polyethylene / polypropylene, linear high density polyethylene / polypropylene, low density polyethylene / polypropylene, binary copolymer of propylene and other α-olefin or terpolymer / polypropylene, linear Examples thereof include high density polyethylene / high density polyethylene, low density polyethylene / high density polyethylene, and the like. In the case of polyolefin resin / polyester resin, for example, polypropylene / polyethylene terephthalate, high-density polyethylene / polyethylene terephthalate, linear high-density polyethylene / polyethylene terephthalate, and low-density polyethylene / polyethylene terephthalate. Moreover, in the case of polyester-type resin / polyester-type resin, copolymer polyester / polyethylene terephthalate etc. are mentioned, for example. Furthermore, the fiber which consists of polyamide-type resin / polyester-type resin, polyolefin-type resin / polyamide-type resin etc. can be illustrated. Among these fibers, the water-permeability imparting agent of the present invention is suitable for polyolefin fibers for producing nonwoven fabrics because the attached water-permeability imparting agent is difficult to fall off by liquids such as urine and body fluids.
繊維の断面構造は鞘芯型、並列型、偏心鞘芯型、多層型、放射型あるいは海島型が例示できるが、繊維製造工程での生産性や、不織布加工の容易さから、偏心を含む鞘芯型または並列型が好ましい。また、断面形状は円形または異形形状とすることができる。異形形状の場合、例えば扁平型、三角形〜八角形等の多角型、Ｔ字型、中空型、多葉型等の任意の形状とすることができる。 The cross-sectional structure of the fiber can be exemplified by a sheath core type, a parallel core type, an eccentric sheath core type, a multilayer type, a radiation type, or a sea island type. A core type or a parallel type is preferred. The cross-sectional shape can be a circular shape or an irregular shape. In the case of an irregular shape, for example, a flat shape, a polygonal shape such as a triangle to an octagon, a T shape, a hollow shape, a multileaf shape, and the like can be used.
本発明の透水性付与剤は、そのまま希釈等せずに繊維本体に付着させてもよく、水等で不揮発分全体の重量割合が０．５〜５重量％となる濃度に希釈してエマルジョンとして繊維本体に付着させてもよい。透水性付与剤を繊維本体へ付着させる工程は、繊維本体の紡糸工程、延伸工程、捲縮工程等のいずれであってもよい。本発明の透水性付与剤を繊維本体に付着させる手段については、特に限定はなく、ローラー給油、ノズルスプレー給油、ディップ給油等の手段を使用してもよい。繊維の製造工程やその特性に合わせ、より均一に効率よく目的の付着量が得られる方法を採用すればよい。また、乾燥の方法としては、熱風および赤外線により乾燥させる方法、熱源に接触させて乾燥させる方法等を用いてよい。 The water-permeability imparting agent of the present invention may be adhered to the fiber main body without being diluted as it is, and diluted with water to a concentration such that the weight ratio of the entire nonvolatile content is 0.5 to 5% by weight as an emulsion. You may make it adhere to a fiber main body. The step of attaching the water permeability imparting agent to the fiber body may be any of a spinning process, a stretching process, a crimping process, and the like of the fiber body. The means for attaching the water permeability imparting agent of the present invention to the fiber body is not particularly limited, and means such as roller lubrication, nozzle spray lubrication, and dip lubrication may be used. A method for obtaining a desired adhesion amount more uniformly and efficiently may be employed in accordance with the fiber manufacturing process and its characteristics. Moreover, as a drying method, you may use the method of drying with a hot air and infrared rays, the method of making it contact with a heat source, and drying.
〔不織布の製造方法〕
また、本発明の不織布の製造方法は、本発明の透水性繊維（例えば短繊維）をカード機等に通し繊維ウェブを作製し、得られた繊維ウェブを熱処理する工程を含むものである。本発明の透水性付与剤は、不織布の製造において繊維ウェブを熱処理する工程を有する場合に、特に好適に使用されるものである。
繊維ウェブを熱処理して接合させる方法としては、加熱ロールまたは超音波によるによる熱圧着、加熱空気による熱融着、熱圧着点（ポイントボンディング）法等の熱融着法が挙げられる。繊維ウェブを熱処理して接合させる一例としては、芯に高融点の樹脂を使用し鞘に低融点の樹脂を使用する鞘芯型の複合繊維の場合、低融点の樹脂の融点付近で熱処理することで、繊維交点の熱接着を容易に行なうことができる。
不織布の製造方法としては、透水性付与剤が付与された短繊維をカード機等に通しスライバーとしたものを上述のように熱処理して接合させ一体化する方法、透水性付与剤が付与された紡績糸や連続糸等を用いて編織加工により編織物としたものを上述のように熱処理して接合させる方法、エアレイド法でパルプ等を積層する際に本発明の透水性繊維（短繊維）と混綿して、上述のように熱処理して接合させる方法等も挙げられる。その他、スパンボンド法、メルトブロー法、フラッシュ紡糸法等により得られた繊維成形体に対して、本発明の透水性付与剤を付着させたものを加熱ロールまたは加熱空気等で熱処理して、または加熱ロールまたは加熱空気等で熱処理したものに本発明の透水性付与剤を付着させて、不織布を製造する方法も挙げられる。
[Method for producing nonwoven fabric]
Moreover, the manufacturing method of the nonwoven fabric of this invention includes the process of passing the water-permeable fiber (for example, short fiber) of this invention through a card machine etc., producing a fiber web, and heat-treating the obtained fiber web. The water-permeability imparting agent of the present invention is particularly preferably used when it has a step of heat-treating the fiber web in the production of the nonwoven fabric.
Examples of the method for joining the fiber webs by heat treatment include thermal fusion methods such as thermocompression using a heated roll or ultrasonic waves, thermal fusion using heated air, and thermocompression bonding (point bonding) method. As an example of heat-bonding the fiber web, in the case of a sheath-core type composite fiber using a high melting point resin for the core and a low melting point resin for the sheath, heat treatment is performed near the melting point of the low melting point resin. Thus, thermal bonding of the fiber intersection can be easily performed.
As a method for producing the nonwoven fabric, a method of heat-treating and joining the short fibers provided with the water permeability imparting agent through a card machine or the like as a sliver as described above, and the water permeability imparting agent were provided. A method in which spun yarns or continuous yarns are used to form a knitted fabric by knitting and heat-treating as described above, and the water-permeable fibers (short fibers) of the present invention when laminating pulp and the like by the airlaid method Examples include a method of blending and heat-bonding and bonding as described above. In addition, a fiber molded body obtained by a spunbond method, a melt blow method, a flash spinning method, or the like is heat-treated with a heating roll or heated air or the like, to which the water permeability imparting agent of the present invention is attached, or heated. A method of manufacturing a nonwoven fabric by attaching the water permeability imparting agent of the present invention to a material heat-treated with a roll or heated air is also included.
スパンボンド法の一例としては、複合繊維樹脂を紡糸し、次に、紡出された複合長繊維フィラメントを冷却流体により冷却し、延伸空気によってフィラメントに張力を加えて所期の繊度とする。その後、紡糸されたフィラメントを捕集ベルト上に捕集し、交絡処理を行ってスパンボンド不織布を得る。接合手段としては、加熱ロールまたは超音波によるによる熱圧着、加熱空気による熱融着、熱圧着点（ポイントボンディング）法等がある。
得られたスパンボンド不織布に本発明の透水性付与剤を付与する方法としては、グラビア法、フレキソ法、ゲートロール法等のロールコーティング法、スプレーコーティング法等で行うことができるが、不織布への塗布量を片面ずつ調節できるものであれば特に限定されるものではない。また、乾燥の方法としては、熱風および赤外線により乾燥させる方法、熱源に接触させて乾燥させる方法等を用いてよい。
As an example of the spunbond method, a composite fiber resin is spun, then the spun composite long fiber filament is cooled with a cooling fluid, and tension is applied to the filament with drawn air to obtain the desired fineness. Thereafter, the spun filament is collected on a collection belt and entangled to obtain a spunbonded nonwoven fabric. Examples of the joining means include thermocompression bonding using a heating roll or ultrasonic waves, heat fusion using heated air, and a thermocompression bonding (point bonding) method.
As a method for imparting the water permeability imparting agent of the present invention to the obtained spunbond nonwoven fabric, it can be performed by a gravure method, a flexo method, a roll coating method such as a gate roll method, a spray coating method, etc. There is no particular limitation as long as the coating amount can be adjusted for each side. Moreover, as a drying method, you may use the method of drying with a hot air and infrared rays, the method of making it contact with a heat source, and drying.
〔透水性繊維の物性〕
本発明の透水性繊維は、液戻り防止性に優れた物性を有している。透水性繊維の液戻り量は、通常１．２ｇ以下、好ましくは１．０ｇ以下、さらに好ましくは０．８ｇ以下、より好ましくは０．６ｇ以下、特に好ましくは０．４ｇ以下、最も好ましくは０．２ｇ以下である。
[Physical properties of water-permeable fibers]
The water-permeable fiber of the present invention has physical properties excellent in liquid return prevention properties. The liquid return amount of the water-permeable fiber is usually 1.2 g or less, preferably 1.0 g or less, more preferably 0.8 g or less, more preferably 0.6 g or less, particularly preferably 0.4 g or less, and most preferably 0. .2 g or less.
本発明の透水性繊維は、耐久透水性に優れている。透水性繊維の耐久透水性評価は、繰り返しの評価が３回目において生理食塩水の消失時間を２０箇所で測定し、消失時間５秒未満となる箇所の個数は、通常１０個以上、好ましくは１２個以上、さらに好ましくは１４個以上、より好ましくは１６個以上、特に好ましくは１８個以上、最も好ましくは２０個である。 The water-permeable fiber of the present invention is excellent in durable water permeability. In the durable water permeability evaluation of the water permeable fiber, the disappearance time of the physiological saline is measured at 20 places in the third evaluation, and the number of places where the disappearance time is less than 5 seconds is usually 10 or more, preferably 12 Or more, more preferably 14 or more, more preferably 16 or more, particularly preferably 18 or more, and most preferably 20.
本発明の透水性繊維は、安全性に優れている。衛生材料用途では、人体に直接接することから、高い安全性が求められている。透水性繊維の安全性評価は、細胞毒性試験結果（ＩＣ５０）を実施し、７０％以上が好ましい。本発明の透水性付与剤を繊維本体に付着させることによって、上記物性が得られる。 The water-permeable fiber of the present invention is excellent in safety. In sanitary material applications, high safety is required because it is in direct contact with the human body. The safety evaluation of the water-permeable fiber is carried out based on a cytotoxicity test result (IC 50 ), and preferably 70% or more. The above physical properties can be obtained by attaching the water permeability imparting agent of the present invention to the fiber body.
以下に本発明を実施例によって説明するが、本発明はこれに限定されるものではない。なお、各実施例および比較例における評価項目と評価方法は以下の通りである。なお、例中の「部」および「％」とあるのは、それぞれ「重量部」および「重量％」を表す。 The present invention will be described below with reference to examples, but the present invention is not limited thereto. In addition, the evaluation items and the evaluation method in each example and comparative example are as follows. In the examples, “parts” and “%” represent “parts by weight” and “% by weight”, respectively.
（実施例１〜１０および比較例１〜１１）
表１および２に示す各成分および水を混合して、透水性付与剤全体に占める不揮発分の重量割合が２０重量％の実施例１〜１０、比較例１〜１１の透水性付与剤をそれぞれ調製した。得られた透水性付与剤をそれぞれ約６０℃の温水で不揮発分の重量割合が１重量％の濃度になるよう希釈して希釈液を得た。また、各希釈液のｐＨ（２０℃）をそれぞれ測定した。結果を表１、２に示す。
次に、繊維本体３００ｇに対しそれぞれの透水性付与剤の希釈液１５０ｇをスプレーで付着させ、透水性繊維に付着する透水性付与剤の付着量を０．５重量％にした。繊維本体は、透水性付与剤等の繊維処理剤が付着していない、ポリプロピレン（芯）−ポリエチレン（鞘）系複合繊維であり、単繊維繊度が１．５Ｄｔｅｘ、繊維長が３８ｍｍのものであった。それぞれの透水性付与剤の希釈液を付着させた繊維を、６０℃の温風乾燥機の中に２時間入れた後、室温で８時間以上放置して乾燥させて、透水性繊維を得た。
(Examples 1-10 and Comparative Examples 1-11)
Each component shown in Tables 1 and 2 and water were mixed, and the water permeability imparting agents of Examples 1 to 10 and Comparative Examples 1 to 11 in which the weight ratio of the nonvolatile content in the entire water permeability imparting agent was 20% by weight, respectively. Prepared. The obtained water-permeability imparting agent was diluted with warm water of about 60 ° C. so that the weight ratio of the nonvolatile content was 1% by weight to obtain a diluted solution. Moreover, pH (20 degreeC) of each dilution liquid was measured, respectively. The results are shown in Tables 1 and 2.
Next, 150 g of a diluted solution of each water permeability imparting agent was attached to the fiber main body 300 g by spraying, so that the amount of the water permeability imparting agent adhering to the water permeable fiber was 0.5% by weight. The fiber body is a polypropylene (core) -polyethylene (sheath) -based composite fiber to which a fiber treatment agent such as a water permeability imparting agent is not attached, and has a single fiber fineness of 1.5 Dtex and a fiber length of 38 mm. It was. The fibers to which the respective liquid permeability imparting agents were attached were placed in a 60 ° C. hot air dryer for 2 hours and then allowed to dry at room temperature for 8 hours or more to obtain water permeable fibers. .
得られた透水性繊維をそれぞれ混打綿工程およびカード試験機を用いたカード工程に通し、目付３０ｇ／ｍ２のウェブを作製した。その際、それぞれの透水性繊維について、下記に示す評価方法でカード工程における物性（カード通過性：シリンダー巻付きおよびスカム発生の有無）を評価した。得られたウェブをエァースルー型熱風循環乾燥機中１３０℃で熱処理してウェブを固定し、不織布を得た。得られた不織布について、下記に示す評価方法で物性（瞬時透水性、耐久透水性および液戻り防止性）をそれぞれ評価した。その結果を表３および４に示す。 The obtained water-permeable fibers were respectively passed through a blended cotton process and a card process using a card testing machine to prepare webs with a basis weight of 30 g / m 2 . At that time, for each water-permeable fiber, the physical properties in the card process (card passing property: presence of cylinder winding and occurrence of scum) were evaluated by the following evaluation method. The obtained web was heat-treated at 130 ° C. in an air-through hot air circulating dryer to fix the web to obtain a nonwoven fabric. About the obtained nonwoven fabric, the physical properties (instant water permeability, durable water permeability, and liquid return prevention property) were evaluated by the evaluation methods shown below. The results are shown in Tables 3 and 4.
〔評価方法〕
（１）シリンダー巻付き
カード試験機を用いて３０℃×７０％ＲＨの条件で試料短繊維４０ｇをカーディングした後にシリンダーを観察し、以下の基準で評価した。なお、５が最も良い評価である。
５…巻付きなし、４…シリンダー面の１／１０に巻付きあり、３…シリンダー面の１／５に巻付きあり、２…シリンダー面の１／３に巻付きあり、１…全面に巻付きあり
〔Evaluation method〕
(1) Cylinder winding The card | curd was observed after carding 40 g of sample short fibers on the conditions of 30 degreeC x 70% RH using the card test machine, and the following references | standards evaluated. Note that 5 is the best evaluation.
5 ... No winding, 4 ... winding to 1/10 of the cylinder surface, 3 ... winding to 1/5 of the cylinder surface, 2 ... winding to 1/3 of the cylinder surface, 1 ... winding to the entire surface With
（２）スカム発生の有無
カード試験機を用いて３０℃×７０％ＲＨの条件で試料短繊維２００ｇをカーディングした後にローラーに付着したスカムを観察し、スカム発生の有無を評価した。
(2) Presence or absence of scum generation After carding 200 g of sample short fibers under a condition of 30 ° C. and 70% RH using a card testing machine, the scum adhering to the roller was observed to evaluate the presence or absence of scum generation.
（３）不織布の瞬時透水性
不織布を濾紙（東洋濾紙、Ｎｏ．５）の上に重ね、不織布表面から１０ｍｍの高さに設置したビューレットより１滴（約０．０５ｍｌ）の生理食塩水を滴下して、不織布表面から水滴が消失するまでの時間を測定する。不織布表面の２０箇所でこの測定を行って５秒未満の個数を表示する。この個数が１８個以上であれば瞬時透水性は良好である。
(3) Instantaneous water permeability of non-woven fabric The non-woven fabric is layered on filter paper (Toyo filter paper, No. 5), and 1 drop (about 0.05 ml) of physiological saline is added from a burette placed at a height of 10 mm from the non-woven fabric surface. It is dripped and the time until water droplets disappear from the nonwoven fabric surface is measured. This measurement is performed at 20 points on the surface of the nonwoven fabric, and the number of less than 5 seconds is displayed. If this number is 18 or more, the instantaneous water permeability is good.
（４）不織布の耐久透水性
不織布（１０ｃｍ×１０ｃｍ）を市販の紙おむつに重ね、その上に内径６０ｍｍの円筒を置き、生理食塩水８０ｍｌを円筒内に注入して不織布を通して紙おむつに吸収させた。注水後３分間放置した後に、不織布を２枚の濾紙（東洋濾紙、Ｎｏ．５）の間に挟み、その上に板（１０ｃｍ×１０ｃｍ）と重り（合計３．５Ｋｇ）を乗せて３分間放置して脱水し、その後さらに５分間風乾した。風乾後の試料不織布に上記円筒内で生理食塩水が通過した箇所について、不織布の瞬時透水性の試験方法によって、生理食塩水の消失時間を２０箇所で測定し、消失時間５秒未満の個数を表示した。この個数が１８個以上であれば耐久透水性は良好である。試験に供した不織布について、同様の作業を繰り返して行う。この繰り返し試験では回数を重ねても生理食塩水の消失個数（消失時間５秒未満となる箇所の個数）が多い方が良い。
(4) Durable water permeability of nonwoven fabric A nonwoven fabric (10 cm × 10 cm) was placed on a commercially available paper diaper, a cylinder with an inner diameter of 60 mm was placed thereon, 80 ml of physiological saline was injected into the cylinder, and the nonwoven fabric was absorbed through the nonwoven fabric. After standing for 3 minutes after water injection, the nonwoven fabric is sandwiched between two filter papers (Toyo Filter Paper, No. 5), and a plate (10 cm × 10 cm) and a weight (total 3.5 kg) are placed on it for 3 minutes. And dehydrated, then air dried for another 5 minutes. About the location where physiological saline passed through the sample nonwoven fabric after air drying in the cylinder, the disappearance time of physiological saline was measured at 20 locations by the instantaneous water permeability test method of the nonwoven fabric, and the number of disappearance time less than 5 seconds was determined. displayed. If this number is 18 or more, the durable water permeability is good. The same operation is repeated for the nonwoven fabric subjected to the test. In this repeated test, it is better that the number of disappearances of the physiological saline (the number of places where the disappearance time is less than 5 seconds) is large even if the number of times is repeated.
（５）不織布の液戻り防止性
市販の紙おむつの上に不織布（１０ｃｍ×１０ｃｍ）を置き、さらにその上に内径６０ｍｍの円筒を置き、生理食塩水１００ｍｌを円筒内に注入して不織布を通して紙おむつに吸収させた。生理食塩水が全て紙おむつに吸収されたら円筒を取り除き、予め秤量した濾紙（東洋濾紙、Ｎｏ．５）を２０枚重ね、これに５Ｋｇの荷重を乗せた。５分間放置後、濾紙の重さを計り、重量増加分を測定して液戻り量（ｇ）とした。１．２ｇ以下を許容範囲としているが、１．０ｇ以下が望ましい。
(5) Liquid return prevention property of nonwoven fabric Place a nonwoven fabric (10 cm x 10 cm) on a commercially available paper diaper, place a cylinder with an inner diameter of 60 mm on it, inject 100 ml of physiological saline into the cylinder, and pass through the nonwoven fabric into the paper diaper. Absorbed. When all the physiological saline was absorbed by the paper diaper, the cylinder was removed, 20 sheets of pre-weighed filter paper (Toyo Filter Paper, No. 5) were stacked, and a 5 kg load was placed thereon. After standing for 5 minutes, the filter paper was weighed and the weight increase was measured to obtain the liquid return amount (g). Although the allowable range is 1.2 g or less, 1.0 g or less is desirable.
（６）細胞毒性試験（ＩＣ５０）
細胞株はＶ７９細胞を用いるコロニー形成法により、水抽出液３〜１００％の濃度範囲で検討し、コロニー形成を５０％阻害する濃度（％）をＩＣ５０とした。抽出条件および処理条件等は「第１５改正 日本薬局方 ２００６年度」のプラスチック製医薬品容器試験法の細胞毒性試験に準拠して実施した。合否の判定は、濃度７０％以上を合格（○）とし、７０％未満を不合格（×）とした。
(6) Cytotoxicity test (IC 50 )
Cell lines by colony formation method using V79 cells were examined in a concentration range of water extract 3 to 100%, and the IC 50 concentration (%) to inhibit colony formation by 50%. Extraction conditions, treatment conditions, and the like were performed in accordance with the cytotoxicity test of the plastic drug container test method of “15th revision Japanese Pharmacopoeia 2006”. In the pass / fail judgment, a density of 70% or more was regarded as acceptable (◯), and a density of less than 70% was regarded as unacceptable (x).
（７）透水性繊維に付着する透水性付与剤の付着率
透水性繊維に付着する透水性付与剤の付着率は、２５℃×４０％ＲＨの温湿度で２４時間調湿した透水性繊維（Ｗ１）を、メタノールを用いて、迅速残脂抽出装置Ｒ−１１型（東海計器（株）製）で抽出し、透水性付与剤付着量（Ｗ２）を求めた。そして下記の式より、透水性付与剤付着率Ｃ％を求めた。
Ｃ＝Ｗ２／Ｗ１×１００（％）
(7) Adhesion rate of water permeability imparting agent adhering to water permeable fiber The adhesion rate of the water permeability imparting agent adhering to the water permeable fiber is a water permeable fiber conditioned at a temperature and humidity of 25 ° C. × 40% RH for 24 hours ( W1) was extracted with methanol using a rapid residual oil extractor R-11 type (manufactured by Tokai Keiki Co., Ltd.) to determine the water permeability imparting agent adhesion amount (W2). And permeation | transmission provision agent adhesion rate C% was calculated | required from the following formula.
C = W2 / W1 × 100 (%)
成分ａ１：オクチルホスフェートカリウム塩
成分ａ２：デシルホスフェートカリウム塩
成分ａ３：ポリオキシエチレン１モルデシルホスフェートカリウム塩
成分ｂ１：ラウリルホスフェートカリウム塩
成分ｂ２：ポリオキシエチレン２モルラウリルホスフェートカリウム塩
成分ｂ３：セチルホスフェートカリウム塩
成分ｃ１：ポリオキシエチレン（２０モル）カスターワックスのマレイン酸縮合物の水酸基を全てベヘン酸で封鎖したエステル
成分ｃ２：ポリオキシエチレン（２０モル）カスターワックスのマレイン酸縮合物の水酸基を全てステアリン酸で封鎖したエステル
成分ｄ１１：ジステアリルジメチルアンモニウムメトサルフェート塩
成分ｄ２１：トリアルキルグリシン誘導体（ビスターＭＳ、松本油脂製薬（株）製）
成分ｄ２２：（ポリ）アルキルアルキレンアミドジアルキルグリシン誘導体（ビスターＣＡＰ、松本油脂製薬（株）製）
成分ｄ３１：ジ椰子アルキルスルホサクシネートＮａ塩
成分ｄ３２：ジトリデシルスルホサクシネートＮａ塩
Component a1: Octyl phosphate potassium salt Component a2: Decyl phosphate potassium salt Component a3: Polyoxyethylene 1 mol decyl phosphate potassium salt component b1: Lauryl phosphate potassium salt component b2: Polyoxyethylene 2 mol lauryl phosphate potassium salt component b3: Cetyl phosphate Potassium salt component c1: Ester component c2: all the hydroxyl groups of maleic acid condensate of polyoxyethylene (20 mol) castor wax blocked with behenic acid All hydroxyl groups of maleic acid condensate of polyoxyethylene (20 mol) castor wax Ester component blocked with stearic acid d 1 1: Distearyldimethylammonium methosulfate salt component d 2 1: Trialkylglycine derivative (Bister MS, manufactured by Matsumoto Yushi Seiyaku Co., Ltd.)
Component d 2 2 :( poly) alkyl polyalkylene amide dialkyl glycine derivatives (Bicester CAP, Matsumoto Yushi-Seiyaku Co., Ltd.)
Component d 3 1: Dicoco alkylsulfosuccinate Na salt Component d 3 2: Ditridecyl sulfosuccinate Na salt
成分ｂ４：ステアリルホスフェートカリウム塩
成分ｃ３：ポリオキシエチレン（２０モル）カスターワックスのマレイン酸縮合物（未封鎖物）
成分ｄ１２：ポリオキシエチレンベヘン酸ジエチレントリアミンのエピクロルヒドリンを反応させたカチオン化物（ポリオキシエチレン基の数：１５）
成分ｄ１３：ポリオキシエチレン（１０モル）ベヘン酸ジエタノールアミド
成分ｅ：ポリオキシエチレン／ポリオキシプロピレン変性シリコーン（Ｓｉ含有率：６５％、ＰＯＥ含有率：１００％、分子量：１００００）。なお、ＰＯＥ含有率は、ポリオキシアルキレン中のポリオキシエチレンの含有率（重量％）を示す。
Component b4: Stearyl phosphate potassium salt Component c3: Maleic acid condensate of polyoxyethylene (20 mol) castor wax (unsealed product)
Component d 12 2: Cationized product of polyoxyethylene behenate diethylenetriamine and epichlorohydrin (number of polyoxyethylene groups: 15)
Component d 13 : Polyoxyethylene (10 mol) behenic acid diethanolamide Component e: Polyoxyethylene / polyoxypropylene-modified silicone (Si content: 65%, POE content: 100%, molecular weight: 10,000). In addition, POE content rate shows the content rate (weight%) of the polyoxyethylene in polyoxyalkylene.
表３から明らかなように、実施例１〜１０の本発明の透水性付与剤を給油した透水性繊維は、カード通過性が良好であり、透水性不織布の瞬時透水性、耐久透水性および液戻り量も少なく良好であった。さらには、細胞毒性試験にも合格した。透水性能の優れた化合物と、ポリオレフィンとの親和性が高い化合物を併用したことで、その相乗効果が良く現れている。この透水性付与剤を付与すれば、繊維に瞬時透水性、耐久透水性、および液戻り防止性を付与し、さらに皮膚への刺激性も低減する事ができ、本発明の効果が確認された。
一方、表４から明らかなように、これらの成分組成範囲から外れる比較例１〜１１は、総ての必要特性を満足することはできなかった。
As is apparent from Table 3, the water-permeable fibers supplied with the water-permeability imparting agent of Examples 1 to 10 have good card permeability, and the instantaneous water-permeability, durable water-permeability and liquid of the water-permeable nonwoven fabric. The return amount was small and good. Furthermore, it passed the cytotoxicity test. The combined use of a compound having excellent water permeability and a compound having a high affinity for polyolefin shows a good synergistic effect. If this water permeability imparting agent is added, the fiber can be given instant water permeability, durable water permeability, and liquid return prevention property, and further the irritation to the skin can be reduced, confirming the effect of the present invention. .
On the other hand, as is clear from Table 4, Comparative Examples 1 to 11 deviating from these component composition ranges could not satisfy all necessary characteristics.
Claims (11)
アルキル基の炭素数が１１〜２２である、アルキルホスフェート塩および／またはポリオキシアルキレン基含有アルキルホスフェート塩（Ｂ）と、
ポリオキシアルキレン基含有ヒドロキシ脂肪酸多価アルコールエステルとジカルボン酸との縮合物の少なくとも１つ以上の水酸基を脂肪酸で封鎖したエステル（Ｃ）とを必須成分として含む透水性付与剤であって、
前記透水性付与剤の不揮発分全体に占める、成分（Ａ）の重量割合が１〜２０重量％、成分（Ｂ）の重量割合が２０〜５０重量％、成分（Ｃ）の重量割合が４１〜６５重量％であり、かつ成分（Ａ）と成分（Ｂ）と成分（Ｃ）の合計の重量割合が８０重量％以上である、透水性付与剤。 An alkyl phosphate salt and / or a polyoxyalkylene group-containing alkyl phosphate salt (A), wherein the alkyl group has 6 to 10 carbon atoms;
An alkyl phosphate salt and / or a polyoxyalkylene group-containing alkyl phosphate salt (B), wherein the alkyl group has 11 to 22 carbon atoms;
A water permeability-imparting agent comprising, as an essential component, an ester (C) obtained by blocking at least one hydroxyl group of a polyoxyalkylene group-containing hydroxy fatty acid polyhydric alcohol ester and a dicarboxylic acid with a fatty acid,
The weight ratio of the component (A) is 1 to 20% by weight, the weight ratio of the component (B) is 20 to 50% by weight, and the weight ratio of the component (C) is 41 to 40%. The water-permeability imparting agent which is 65% by weight and the total weight ratio of the component (A), the component (B) and the component (C) is 80% by weight or more.
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| JP6959748B2 (en) * | 2017-03-17 | 2021-11-05 | 東邦化学工業株式会社 | Water permeable agent |
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| R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
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| R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |