JP2021042498A - Antibacterial agent for high-pressure process of fiber and method for high-pressure antibacterial process of fiber - Google Patents
Antibacterial agent for high-pressure process of fiber and method for high-pressure antibacterial process of fiber Download PDFInfo
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- 239000000835 fiber Substances 0.000 title claims abstract description 74
- 230000000844 anti-bacterial effect Effects 0.000 title claims abstract description 54
- 239000003242 anti bacterial agent Substances 0.000 title claims abstract description 37
- 238000000034 method Methods 0.000 title abstract description 26
- KYGZCKSPAKDVKC-UHFFFAOYSA-N Oxolinic acid Chemical compound C1=C2N(CC)C=C(C(O)=O)C(=O)C2=CC2=C1OCO2 KYGZCKSPAKDVKC-UHFFFAOYSA-N 0.000 claims abstract description 26
- 229960000321 oxolinic acid Drugs 0.000 claims abstract description 25
- 150000003839 salts Chemical class 0.000 claims abstract description 23
- 229920000728 polyester Polymers 0.000 claims abstract description 11
- 239000004480 active ingredient Substances 0.000 claims abstract description 3
- 238000012545 processing Methods 0.000 claims description 36
- 238000011282 treatment Methods 0.000 claims description 23
- 238000009931 pascalization Methods 0.000 claims description 16
- 238000003672 processing method Methods 0.000 claims description 12
- 239000007788 liquid Substances 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 5
- 239000002245 particle Substances 0.000 claims description 5
- 229920006304 triacetate fiber Polymers 0.000 claims description 5
- 229910052751 metal Inorganic materials 0.000 claims description 3
- 239000002184 metal Substances 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 229920002994 synthetic fiber Polymers 0.000 abstract description 14
- 239000012209 synthetic fiber Substances 0.000 abstract description 12
- 239000011230 binding agent Substances 0.000 abstract description 10
- 229920006221 acetate fiber Polymers 0.000 abstract description 2
- 238000004043 dyeing Methods 0.000 description 23
- 239000004753 textile Substances 0.000 description 14
- 238000005406 washing Methods 0.000 description 9
- 239000006185 dispersion Substances 0.000 description 6
- 241000191967 Staphylococcus aureus Species 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- 238000010998 test method Methods 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- 241000588747 Klebsiella pneumoniae Species 0.000 description 4
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 4
- 230000002411 adverse Effects 0.000 description 4
- 238000003287 bathing Methods 0.000 description 4
- 239000000975 dye Substances 0.000 description 4
- 239000011701 zinc Substances 0.000 description 4
- 229910052725 zinc Inorganic materials 0.000 description 4
- 238000004140 cleaning Methods 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 229910021645 metal ion Inorganic materials 0.000 description 3
- 241000894006 Bacteria Species 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 230000006866 deterioration Effects 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000011156 evaluation Methods 0.000 description 2
- 239000004744 fabric Substances 0.000 description 2
- 239000000575 pesticide Substances 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 238000009987 spinning Methods 0.000 description 2
- ILJSQTXMGCGYMG-UHFFFAOYSA-N triacetic acid Chemical compound CC(=O)CC(=O)CC(O)=O ILJSQTXMGCGYMG-UHFFFAOYSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 229920000742 Cotton Polymers 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 229910052784 alkaline earth metal Inorganic materials 0.000 description 1
- -1 alkaline earth metal salts Chemical class 0.000 description 1
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical class [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 description 1
- 229940088710 antibiotic agent Drugs 0.000 description 1
- 229940121375 antifungal agent Drugs 0.000 description 1
- 239000003429 antifungal agent Substances 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 239000003899 bactericide agent Substances 0.000 description 1
- 159000000007 calcium salts Chemical class 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 239000000986 disperse dye Substances 0.000 description 1
- GRWZHXKQBITJKP-UHFFFAOYSA-L dithionite(2-) Chemical compound [O-]S(=O)S([O-])=O GRWZHXKQBITJKP-UHFFFAOYSA-L 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 238000004898 kneading Methods 0.000 description 1
- 159000000003 magnesium salts Chemical class 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- LISFMEBWQUVKPJ-UHFFFAOYSA-N quinolin-2-ol Chemical compound C1=CC=C2NC(=O)C=CC2=C1 LISFMEBWQUVKPJ-UHFFFAOYSA-N 0.000 description 1
- 125000002943 quinolinyl group Chemical group N1=C(C=CC2=CC=CC=C12)* 0.000 description 1
- 238000009958 sewing Methods 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- 238000010186 staining Methods 0.000 description 1
- 239000011550 stock solution Substances 0.000 description 1
- 239000002759 woven fabric Substances 0.000 description 1
- 150000003751 zinc Chemical class 0.000 description 1
Classifications
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/322—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing nitrogen
- D06M13/35—Heterocyclic compounds
- D06M13/355—Heterocyclic compounds having six-membered heterocyclic rings
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
- A01N25/02—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests containing liquids as carriers, diluents or solvents
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
- A01N43/90—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having two or more relevant hetero rings, condensed among themselves or with a common carbocyclic ring system
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M16/00—Biochemical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. enzymatic
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/02—Natural fibres, other than mineral fibres
- D06M2101/04—Vegetal fibres
- D06M2101/06—Vegetal fibres cellulosic
- D06M2101/08—Esters or ethers of cellulose
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/16—Synthetic fibres, other than mineral fibres
- D06M2101/30—Synthetic polymers consisting of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M2101/32—Polyesters
Abstract
Description
本発明は、ポリエステル繊維等の合成繊維類、アセテート繊維等の半合成繊維類、天然繊維、及び合成繊維、半合成繊維類と天然繊維類との混合繊維からなる繊維製品に抗菌性等を付与する抗菌剤、さらに、その抗菌剤を用いた繊維製品の抗菌加工方法に関する。 The present invention imparts antibacterial properties to synthetic fibers such as polyester fibers, semi-synthetic fibers such as acetate fibers, natural fibers, and textile products composed of synthetic fibers and mixed fibers of semi-synthetic fibers and natural fibers. The present invention relates to an antibacterial agent, and an antibacterial processing method for textile products using the antibacterial agent.
特に、本発明は、結合剤を使用することなく、繊維製品に耐久性のある黄色ブドウ球菌、肺炎桿菌等に対する抗菌性を付与する繊維類の高圧加工処理用抗菌剤及び繊維類の高圧抗菌加工方法に関する。 In particular, the present invention provides antibacterial agents for high-pressure processing of fibers and high-pressure antibacterial processing of fibers that impart antibacterial properties to textile products such as Staphylococcus aureus and Klebsiella pneumoniae without using a binder. Regarding the method.
近年、医療施設で使用される白衣、シーツ等に限らず、靴下、下着等の衣料用繊維製品、カーテン、タオル、カーペット等の身のまわりの繊維製品に、抗菌加工された繊維が使用されるようになってきている。しかし、抗菌加工では、通常、抗菌効果の持続性を高めるために、結合剤で処理することが一般的に行われている。また、繊維製品の場合、抗菌加工だけでなく、多くは難燃化、染色等の他の加工処理も行われるのが通常であり、その場合には他の処理との関係で加工条件、加工順序等色々な制約を受けることも多いのが現状である。
しかし、上述の結合剤による処理は、繊維の風合いを損ねたり、抗菌性能の低下といった問題が生じることがあり、その改善が求められている。また、抗菌加工以外の処理をそれぞれ別工程で行うことは作業工程上好ましいことではなく、いくつかの処理を同時に行うこと、例えば、染色と抗菌加工などを同時に行うことが可能な加工方法も強く望まれている。
さらに、繊維製品は洗濯をすることが前提となるため、抗菌加工では結合剤での処理によらず、耐洗濯性を備えることも要求されている。
In recent years, antibacterial processed fibers have been used not only for white coats and sheets used in medical facilities, but also for textile products for clothing such as socks and underwear, and textile products around us such as curtains, towels and carpets. It is becoming like. However, in antibacterial processing, it is common to treat with a binder in order to enhance the durability of the antibacterial effect. In the case of textile products, not only antibacterial processing but also other processing such as flame retardancy and dyeing is usually performed. In that case, processing conditions and processing are performed in relation to other processing. The current situation is that there are many restrictions such as the order.
However, the treatment with the above-mentioned binder may cause problems such as impairing the texture of the fiber and deterioration of the antibacterial performance, and improvement thereof is required. In addition, it is not preferable in terms of work process to perform treatments other than antibacterial processing in separate processes, and a processing method capable of performing several treatments at the same time, for example, dyeing and antibacterial processing at the same time, is also strong. It is desired.
Further, since textile products are premised on being washed, antibacterial processing is also required to have washing resistance regardless of treatment with a binder.
合成繊維等からなる製品の抗菌加工技術としては、その紡糸原液に抗菌剤を練り込み、紡糸して抗菌特性を有する繊維を使用する方法、普通に紡糸された合成、半合成繊維又はそれらを縫製して得た製品に抗菌剤を結合剤と共に付着させる方法が代表的なものである。本発明の高圧加工処理用抗菌剤は、他の抗菌剤とは異なり、結合剤を用いずに繊維に強固に付着可能であり、また、染色浴で染料と共存することができ、繊維又は繊維製品に対し、染色と同時に抗菌剤を付着させることも可能であるため、染色同浴加工に有利に使用することができる。 Antibacterial processing technology for products made of synthetic fibers, etc. includes a method of kneading an antibacterial agent into the spinning stock solution and spinning to use fibers having antibacterial properties, ordinary spun synthetic fibers, semi-synthetic fibers, or sewing them. A typical method is to attach an antibacterial agent together with a binder to the product thus obtained. Unlike other antibacterial agents, the antibacterial agent for high-pressure processing of the present invention can firmly adhere to fibers without using a binder, and can coexist with dyes in a dyeing bath, and the fibers or fibers can coexist. Since it is possible to attach an antibacterial agent to the product at the same time as dyeing, it can be advantageously used for dyeing and bathing.
結合剤を用いずに繊維類に強固に付着でき、また、染色同浴加工に使用可能な抗菌剤としては、現時点では、特許文献１に記載されているピリチオン亜鉛が唯一実用可能なものとして知られている。また、そのピリチオン亜鉛を用いた加工方法には、繊維や繊維製品を抗菌剤を含む染色浴に浸漬し加圧下に保持する方法、繊維や繊維製品に抗菌剤を含む処理液を含浸させ次いで加熱する方法等が、特許文献１で提案されている。 At present, pyrithion zinc described in Patent Document 1 is known to be the only practical antibacterial agent that can be firmly attached to fibers without using a binder and can be used for dyeing and bathing. Has been done. The processing method using pyrithion zinc includes a method of immersing fibers and textile products in a dyeing bath containing an antibacterial agent and holding them under pressure, and a method of impregnating fibers and textile products with a treatment liquid containing an antibacterial agent and then heating. A method of doing so is proposed in Patent Document 1.
しかし、上記特許文献１で使用する抗菌剤は、その化学構造中に亜鉛金属イオンを含むものであるため、製造工程や抗菌加工処理時には厳密なｐＨ管理も必要であり、また、鉄
や銅成分が存在する環境下ではその抗菌剤を製造することも、使用することもできないという問題点がある。さらに、同様の理由から、染色同浴加工に用いる場合は使用できる染料に制限がある。
また、上記特許文献１の抗菌剤は、染色同浴加工に用いた場合、耐光堅牢度などの染色性能に悪影響を及ぼすこともあり、抗菌性能と共に染色性能も改善することができ、さらに、染色同浴加工にも使用できる抗菌剤の開発が繊維加工の分野で強く求められている現状である。
However, since the antibacterial agent used in Patent Document 1 contains zinc metal ions in its chemical structure, strict pH control is required during the manufacturing process and antibacterial processing, and iron and copper components are present. There is a problem that the antibacterial agent cannot be manufactured or used in such an environment. Furthermore, for the same reason, there are restrictions on the dyes that can be used when used for dyeing and bathing.
Further, when the antibacterial agent of Patent Document 1 is used for dyeing bath processing, it may adversely affect the dyeing performance such as light fastness, and the dyeing performance can be improved as well as the antibacterial performance, and further, the dyeing performance can be improved. Currently, there is a strong demand in the field of textile processing for the development of antibacterial agents that can also be used in the same bath processing.
以上のとおり、繊維加工分野で使用する抗菌剤には、単に一般的な抗菌性能だけでなく、繊維評価技術協議会で規定する特定制菌加工、耐洗濯性、更には染色が必要な場合に染色同浴加工にも使用でき、染色性能にも悪影響を与えない新しい染色・抗菌加工技術の開発が待たれている。 As described above, antibacterial agents used in the field of textile processing require not only general antibacterial performance but also specific antibacterial processing, washing resistance, and dyeing specified by the Fiber Evaluation Technology Council. Development of new dyeing / antibacterial processing technology that can be used for dyeing bath processing and does not adversely affect dyeing performance is awaited.
本発明者等は、結合剤を用いることなく耐久性のある抗菌性能を維持でき、また、染色同浴加工にも使用できる抗菌剤及び抗菌加工方法について精力的に研究を行い、これらの研究の中から、極めて有効な高圧加工処理用抗菌剤及び高圧抗菌加工方法を見出し、本発明の完成に至ったものである。
本発明は、主に、合成繊維類を主体とする繊維類に対し、結合剤を用いることなく、黄色ブドウ球菌等に対して強い抗菌性能を持続でき、耐洗濯性を付与できる繊維類の高圧加工処理用抗菌剤及び繊維類の抗菌加工方法を提供することを目的とするものである。さらに本発明の抗菌剤は、染色同浴加工にも使用できるものである。
The present inventors have energetically researched antibacterial agents and antibacterial processing methods that can maintain durable antibacterial performance without using a binder and can also be used for dyeing bath processing. Among them, an extremely effective antibacterial agent for high-pressure processing and a high-pressure antibacterial processing method have been found, and the present invention has been completed.
In the present invention, the high pressure of the fiber which can maintain strong antibacterial performance against Staphylococcus aureus and the like and impart washing resistance mainly to the fiber mainly composed of synthetic fiber without using a binder. It is an object of the present invention to provide an antibacterial agent for processing and an antibacterial processing method for fibers. Further, the antibacterial agent of the present invention can also be used for dyeing and bathing.
本発明は、以下の高圧加工処理用抗菌剤及びその抗菌剤を使用する繊維類の高圧抗菌加工方法に関する発明である。
（１）オキソリニック酸又はその塩を有効成分として含有し、高圧加工処理で使用されることを特徴とする繊維類の高圧加工処理用抗菌剤、
（２）前記オキソリニック酸の塩が二価以上の金属塩であることを特徴とする（１）に記載の繊維類の高圧加工処理用抗菌剤、
（３）オキソリニック酸又はその塩の粒径が０．１〜１０ミクロンであることを特徴とする前記（１）又は（２）に記載の繊維類の高圧加工処理用抗菌剤、
（４）オキソリニック酸又はその塩及び水の存在下、オキソリニック酸又はその塩の濃度が０．０１〜１０重量％である抗菌加工処理液に繊維類を浸漬し、加圧下、６０〜１５０℃の処理浴中で加熱処理することを特徴とする繊維類の高圧抗菌加工方法、
（５）前記処理液がさらに染料を含むことを特徴とする前記（４）に記載の繊維類の高圧抗菌加工方法、
（６）前記繊維がポリエステル繊維又はトリアセテート繊維であることを特徴とする（４）又は（５）に記載の繊維類の高圧抗菌加工方法。
The present invention relates to the following antibacterial agent for high-pressure processing and a method for high-pressure antibacterial processing of fibers using the antibacterial agent.
(1) An antibacterial agent for high-pressure processing of fibers, which contains oxolinic acid or a salt thereof as an active ingredient and is used in high-pressure processing.
(2) The antibacterial agent for high-pressure processing of fibers according to (1), wherein the salt of the oxolinic acid is a metal salt having a divalent value or higher.
(3) The antibacterial agent for high-pressure processing of fibers according to (1) or (2) above, wherein the particle size of oxolinic acid or a salt thereof is 0.1 to 10 microns.
(4) In the presence of oxolinic acid or a salt thereof and water, the fibers are immersed in an antibacterial processing solution having a concentration of oxolinic acid or a salt thereof of 0.01 to 10% by weight, and the fibers are immersed under pressure at 60 to 150 ° C. High-pressure antibacterial processing method for fibers, which is characterized by heat treatment in a treatment bath.
(5) The high-pressure antibacterial processing method for fibers according to (4) above, wherein the treatment liquid further contains a dye.
(6) The high-pressure antibacterial processing method for fibers according to (4) or (5), wherein the fiber is a polyester fiber or a triacetate fiber.
本発明によれば、抗菌性能、処理効率が極めて高く、染色性能にも悪影響を与えない極めて優れた高圧加工処理用抗菌剤及び処理方法が提供される。特に、ポリエステル、トリアセテートといった人造繊維製品及びこれらと天然繊維との混合繊維製品に対して黄色ブドウ球菌、肺炎桿菌等の細菌に対して優れた抗菌性を発揮する加工処理を施すことができ、付与された抗菌性能は、洗濯にも十分耐えるものであり、それらの効果は金属イオンの存在にも影響を受けない。 According to the present invention, an extremely excellent antibacterial agent and treatment method for high-pressure processing, which have extremely high antibacterial performance and treatment efficiency and do not adversely affect dyeing performance, are provided. In particular, artificial fiber products such as polyester and triacetate and mixed fiber products of these and natural fibers can be processed to exhibit excellent antibacterial properties against bacteria such as Staphylococcus aureus and Klebsiella pneumoniae. The antibacterial performance is sufficiently resistant to washing, and their effects are not affected by the presence of metal ions.
以下、本発明を詳細に説明する。 Hereinafter, the present invention will be described in detail.
本発明の処理方法を用い得る繊維類としては、木綿等の天然繊維、ポリエステル繊維等の合成繊維、トリアセテート繊維等の半合成繊維類及びこれらを混合した繊維を挙げることができるが、その中ではポリエステル繊維又はトリアセテート繊維を好ましく使用することができる。 Examples of the fibers that can use the treatment method of the present invention include natural fibers such as cotton, synthetic fibers such as polyester fibers, semi-synthetic fibers such as triacetate fibers, and fibers in which these are mixed. Polyester fiber or triacetate fiber can be preferably used.
繊維の形態としては、糸、編物、織物、布が挙げられ、製品としては例えば衣料品、寝装寝具、敷物、カーテン、屋内壁布、タオル、布巾等の製品が挙げられる。
本発明で使用する高圧加工処理用抗菌・抗カビ剤としては、オキソリニック酸又はその塩が用いられる。
Examples of the form of the fiber include threads, knitted fabrics, woven fabrics, and cloths, and examples of products include products such as clothing, bedding, rugs, curtains, indoor wall cloths, towels, and cloths.
As the antibacterial / antifungal agent for high-pressure processing used in the present invention, oxolinic acid or a salt thereof is used.
本発明において用いられるオキソリニック酸は、化学名が５-エチル-５，８-ジヒドロ-８-オキソ［１，３］ジオキソロ［４，５-ｇ］キノリン-７-カルボン酸であり、The Pesticide Manual第１０版(British Crop Protection Council発行) 、第７６０頁に記載の抗菌性化合物であり、本発明においては抗菌活性を有するオキソリニック酸だけでなく、その任意の塩、例えば、カルシウム塩、マグネシウム塩等のアルカリ土類金属塩、亜鉛塩、アルミニウム塩などの二価以上の金属塩の形でも使用される。 The oxolinic acid used in the present invention has a chemical name of 5-ethyl-5,8-dihydro-8-oxo [1,3] dioxolo [4,5-g] quinoline-7-carboxylic acid and is the Pesticide Manual. The 10th edition (published by the British Crop Protection Council), page 760, is an antibacterial compound, and in the present invention, not only an oxolinic acid having an antibacterial activity but also any salt thereof, for example, a calcium salt, a magnesium salt, etc. It is also used in the form of more than divalent metal salts such as alkaline earth metal salts, zinc salts and aluminum salts.
オキソリニック酸は、キノリン骨格を有する抗菌剤（殺菌剤）であり、農薬としても使用されている化合物である。また、獣医学領域では、キノロン系抗生物質の一つとして利用され、安全性の評価も実施されている。
本発明のオキソリニック酸又はその塩の平均粒径は、取り扱い性や分散性の観点から０．１〜１０ミクロンであることが好ましい。
Oxolinic acid is an antibacterial agent (bactericidal agent) having a quinoline skeleton and is a compound that is also used as a pesticide. In the field of veterinary medicine, it is used as one of the quinolone antibiotics and its safety is being evaluated.
The average particle size of the oxolinic acid of the present invention or a salt thereof is preferably 0.1 to 10 microns from the viewpoint of handleability and dispersibility.
本発明による繊維類の抗菌加工処理は加圧下に処理を行うものであり、耐圧密閉容器中に、被加工繊維重量に対し、高圧加工処理用抗菌剤０．０１〜１０重量％程度、好ましくは０．１〜５重量％になるようにオキソリニック酸又はその塩を入れ、これに繊維類を浸し、４０〜２００℃で加熱処理することが好ましく、より好ましくは６０〜１５０℃である。処理時間は通常、１０〜６０分間程度である。また、加圧条件は、常圧程度の１０１３ｈＰａから４８００ｈＰａ程度以下の範囲であることが好ましい。オキソリニック酸又はその塩の濃度、処理温度、処理時間が上記範囲であれば、繊維類に対し十分な抗菌性能を付与することができる。染色同浴加工処理の場合は、処理液中の染料濃度は、０．０１〜１０重量％程度である。 The antibacterial processing treatment of fibers according to the present invention is performed under pressure, and the antibacterial agent for high-pressure processing treatment is preferably about 0.01 to 10% by weight, preferably about 0.01 to 10% by weight, based on the weight of the fiber to be processed in a pressure-resistant airtight container. It is preferable to add oxolinic acid or a salt thereof so as to be 0.1 to 5% by weight, soak the fibers in the oxolinic acid, and heat-treat at 40 to 200 ° C., more preferably 60 to 150 ° C. The processing time is usually about 10 to 60 minutes. Further, the pressurizing condition is preferably in the range of about 1013 hPa to about 4800 hPa or less, which is about normal pressure. If the concentration of oxolinic acid or a salt thereof, the treatment temperature, and the treatment time are within the above ranges, sufficient antibacterial performance can be imparted to the fibers. In the case of the dyeing same bath processing treatment, the dye concentration in the treatment liquid is about 0.01 to 10% by weight.
上記のオキソリニック酸又はその塩を分散液として使用する場合は、分散液は取り扱いの安定性等からオキソリニック酸又はその塩の濃度を１０〜８０重量％としておき、実際に繊維加工に用いる場合は、用途目的に応じ、適当に希釈して用いる。通常は浴中では加工液中のオキソリニック酸又はその塩が被加工繊維重量に対し０．０１〜１０重量％程度の濃度になるように希釈して用いるのが良い。 When the above-mentioned oxolinic acid or a salt thereof is used as a dispersion liquid, the concentration of the oxolinic acid or a salt thereof is set to 10 to 80% by weight in the dispersion liquid from the viewpoint of handling stability, etc., and when actually used for fiber processing, It is used after being appropriately diluted according to the purpose of use. Usually, in a bath, it is preferable to dilute the oxolinic acid in the processing liquid or a salt thereof so as to have a concentration of about 0.01 to 10% by weight with respect to the weight of the fiber to be processed.
前記の処理方法において処理後、さらに、熱処理を行うことにより、耐洗濯性、即ち、洗濯による抗菌性の劣化防止効力を高めることができる。この熱処理は、通常、繊維を１１０〜２００℃、好ましくは１００〜１５０℃で０．５〜３分間程度、保持することにより行われる。 By further performing heat treatment after the treatment in the above-mentioned treatment method, the washing resistance, that is, the effect of preventing deterioration of the antibacterial property due to washing can be enhanced. This heat treatment is usually carried out by holding the fibers at 110 to 200 ° C., preferably 100 to 150 ° C. for about 0.5 to 3 minutes.
繊維類の抗菌加工は繊維の種類によって条件が多少変わるが、ポリエステル繊維の場合は加圧下、１１０〜１４０℃程度の温度で、トリアセテート繊維の場合は常圧下、６０〜１００℃程度の温度で処理することが望ましい。いずれの場合も処理時間は１０分から１時間程度でよい。 The conditions for antibacterial processing of fibers vary slightly depending on the type of fiber, but polyester fibers are treated at a temperature of about 110 to 140 ° C under pressure, and triacetate fibers are treated at a temperature of about 60 to 100 ° C under normal pressure. It is desirable to do. In either case, the processing time may be about 10 minutes to 1 hour.
このようにすることにより、本発明のオキソリニック酸又はその塩は、良好に繊維類の
繊維分子間に入り込み旨く固定され、抗菌性能の持続性が向上する。
By doing so, the oxolinic acid of the present invention or a salt thereof is satisfactorily inserted between the fiber molecules of the fibers and fixed well, and the sustainability of the antibacterial performance is improved.
次に、実施例により、本発明を更に具体的に説明するが、本発明はこれら実施例に限定されるものではない。
なお、実施例中の、洗濯法や各種試験方法は、次の方法に従った。
１．洗濯法
繊維評価技術協議会「ＳＥＫマーク繊維製品の洗濯方法」に準じた。
Next, the present invention will be described in more detail with reference to Examples, but the present invention is not limited to these Examples.
The washing method and various test methods in the examples followed the following methods.
1. 1. Washing method
According to the Textile Evaluation Technology Council "Washing Method for SEK Mark Textile Products".
２．抗菌性試験
１）試験方法 ＪＩＳ Ｌ１９０２「繊維製品の抗菌性試験方法及び抗菌効果」に準じた
。
２）供試菌株
黄色ブドウ球菌（Ｓｔａｐｈｙｌｏｃｏｃｃｕｓ ａｕｒｅｕｓ）
肺炎桿菌（Ｋｌｅｂｓｉｅｌｌａ ｐｎｅｕｍｏｎｉａｅ）
2. Antibacterial test 1) Test method JIS L1902 "Antibacterial test method and antibacterial effect of textile products" was followed.
2) Test strain Staphylococcus aureus
Klebsiella pneumoniae
３．耐光堅牢度試験
試験方法 ＪＩＳ Ｌ０８４２「紫外線カーボンアーク灯光に対する染色堅ろう度試験
方法」に準じた。
3. 3. Light fastness test Test method JIS L0842 "Dyeing fastness test method for ultraviolet carbon arc lamp light" was followed.
実施例
ポリエステル標準布（トロピカル１３５ｇ／ｍ２：谷頭商店）を用い、下記の条件で試験試料を作成した。
加工機：１２色回転ポット染色試験機（MINI-COLOUR 12EL型：（株）テクサム技研製）
加工液：オキソリニック酸分散液（固型分１０％，平均粒径１ミクロン）
分散染料（Kayalon Polyester Navy Blue EX-SF 200：日本化薬（株））2.25%
owf
染色酸（ウルトラN-2：大和化学工業（株））0.5g／ｌ
均染剤（イオネットRAP-250：三洋化成工業（株））0.5g／ｌ
浴比： １：１５
加工温度及び時間： １３０℃×３０分間。加工後、湯洗，脱水を行った。
還元洗浄
洗浄液：ハイドロサルファイト（試薬）2g／ｌ
炭酸ソーダ（試薬）2g／ｌ
還元剤（ダイソーパーRC-150：大和化学工業（株））1g／ｌ
浴比： １：１５
洗浄温度及び時間： ８０℃×２０分間。
Example Using a polyester standard cloth (Tropical 135 g / m 2 : Tanito Shoten), a test sample was prepared under the following conditions.
Processing machine: 12-color rotary pot dyeing tester (MINI-COLOUR 12EL type: manufactured by Texam Giken Co., Ltd.)
Processing liquid: Oxolinic acid dispersion liquid (solid form 10%, average particle size 1 micron)
Disperse dye (Kayalon Polyester Navy Blue EX-SF 200: Nippon Kayaku Co., Ltd.) 2.25%
owf
Staining acid (Ultra N-2: Daiwa Chemical Industry Co., Ltd.) 0.5 g / l
Leveling agent (Ionet RAP-250: Sanyo Chemical Industries, Ltd.) 0.5 g / l
Bath ratio: 1:15
Processing temperature and time: 130 ° C x 30 minutes. After processing, it was washed with hot water and dehydrated.
Reduction cleaning cleaning solution: Hydrosulfite (reagent) 2 g / l
Sodium carbonate (reagent) 2 g / l
Reducing agent (Daisoper RC-150: Daiso Chemical Industry Co., Ltd.) 1 g / l
Bath ratio: 1:15
Cleaning temperature and time: 80 ° C x 20 minutes.
比較例
上記実施例のオキソリニック酸分散液の代わりにピリチオン亜鉛分散液（固型分６０％，平均粒径１ミクロン）を加工、比較用試験試料を作成した。
Comparative Example A pyrithion zinc dispersion (solid form 60%, average particle size 1 micron) was processed in place of the oxolinic acid dispersion of the above example to prepare a comparative test sample.
実施例、比較例で使用した抗菌成分分散液１００ｍｌに金属イオンを含む水溶液１ｍｌを添加、状態の変化を確認した。 1 ml of an aqueous solution containing metal ions was added to 100 ml of the antibacterial component dispersion used in Examples and Comparative Examples, and changes in the state were confirmed.
本発明によれば、抗菌性能、処理効率が極めて高く、染色性能にも悪影響を与えない極めて優れた高圧加工処理用抗菌剤及び処理方法が提供される。特に、ポリエステル、トリアセテートといった人造繊維製品及びこれらと天然繊維との混合繊維製品に対して黄色ブドウ球菌、肺炎桿菌等の細菌に対して優れた抗菌性を発揮する加工処理を施すことができる。 According to the present invention, an extremely excellent antibacterial agent and treatment method for high-pressure processing, which have extremely high antibacterial performance and treatment efficiency and do not adversely affect dyeing performance, are provided. In particular, artificial fiber products such as polyester and triacetate and mixed fiber products of these and natural fibers can be subjected to a processing treatment that exhibits excellent antibacterial properties against bacteria such as Staphylococcus aureus and Klebsiella pneumoniae.
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