JP2021042488A - Water-repellent fabric and method for producing the same - Google Patents
Water-repellent fabric and method for producing the same Download PDFInfo
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- 229920000877 Melamine resin Polymers 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
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Images
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- Chemical Or Physical Treatment Of Fibers (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
Abstract
Description
本発明は、撥水性布帛及びその製造方法に関する。 The present invention relates to a water repellent fabric and a method for producing the same.
従来、レインコートやダウンジャケットなどのアパレル製品において、防汚・防水の観点から、撥水性が良好であり、かつ、洗濯耐久性をも有する撥水性布帛の開発が望まれている。また、近年、地球環境や作業環境の保護を目的に、VOC規制等の有機溶剤排出規制が制定されたことに鑑み、できるだけ環境への負荷が小さいプロセスでの加工が望まれている。
繊維製品における従来の一般的な撥水加工では、フッ素系共重合物に代表される疎水性物質を主成分とする撥水剤の被膜を、布帛を構成する繊維表面に形成することで、布帛の表面張力を低減させ、撥水性を付与している。より良好な撥水性を付与するためには、布帛の表面張力を低減させることに加え、被膜に適切な凹凸形状を形成することにより、蓮の葉効果を発現させることが有効である。
Conventionally, in apparel products such as raincoats and down jackets, it has been desired to develop a water-repellent fabric having good water repellency and washing durability from the viewpoint of antifouling and waterproofing. Further, in view of the fact that organic solvent emission regulations such as VOC regulations have been enacted in recent years for the purpose of protecting the global environment and working environment, processing in a process that has as little environmental impact as possible is desired.
In the conventional general water-repellent treatment of textile products, a film of a water-repellent agent containing a hydrophobic substance typified by a fluorocopolymer as a main component is formed on the surface of the fibers constituting the fabric. The surface tension of the fabric is reduced and water repellency is imparted. In order to impart better water repellency, it is effective to exhibit the lotus leaf effect by forming an appropriate uneven shape on the coating film in addition to reducing the surface tension of the fabric.
先行研究においては、より高い撥水性を有する布帛を提供するために、ナノ粒子を用いて凹凸形状を有する被膜を繊維基布上に形成する手法に関して、多数の研究が行われている。
例えば、以下の特許文献１では、アセトンに疎水性シリカ微粒子及びバインダー樹脂を分散させた液を繊維基材表面に噴霧することにより、布帛表面にナノオーダーの凹凸を有する疎水性被膜を形成し、撥水性を付与している。
また、以下の特許文献２では、疎水性無機微粒子と撥水剤の水分散体を繊維基材に浸漬させた後に熱処理することにより、繊維基材表面に疎水性シリカと撥水剤からなる被膜を形成し、撥水性を付与している。
また、以下の特許文献３では、エタノールに疎水性シリカ微粒子を分散させた分散液を繊維基材に塗布して乾燥させ、基布表面を疎水性シリカ微粒子で被覆することにより、撥水性を発現させている。
さらに、以下の特許文献４では、アルコール、アルコキシシラン、パーフルオロアルキルシラン、親水性又は疎水性シリカ微粒子、アルコキシシランの加水分解を促進する触媒、及び水からなるコーティング組成物を繊維基材に浸漬させ、乾燥させる工程を繰り返すことで、基材表面に粒子と疎水性物質を積層させた撥水性被膜を形成している。
In previous studies, many studies have been conducted on a method of forming a film having an uneven shape on a fiber-based fabric using nanoparticles in order to provide a fabric having higher water repellency.
For example, in Patent Document 1 below, a solution in which hydrophobic silica fine particles and a binder resin are dispersed in acetone is sprayed onto the surface of a fiber base material to form a hydrophobic film having nano-order irregularities on the surface of the fabric. Gives water repellency.
Further, in
Further, in
Further, in Patent Document 4 below, a coating composition consisting of alcohol, alkoxysilane, perfluoroalkylsilane, hydrophilic or hydrophobic silica fine particles, a catalyst for promoting hydrolysis of alkoxysilane, and water is immersed in a fiber base material. By repeating the steps of causing and drying, a water-repellent film in which particles and a hydrophobic substance are laminated is formed on the surface of the base material.
これらの技術では、多様な方法を用いて繊維基材に対して凹凸を有する撥水性被膜を形成し、高い撥水性を付与することに成功している。しかしながら、加工液中に疎水性粒子を分散させるために多量の有機溶媒を使用する必要があり、環境負荷低減の観点からは望ましくない。
また、前記した特許文献のいずれにおいても、洗濯耐久性向上のための具体的な技術的手段の開示はない。
In these techniques, various methods have been used to form a water-repellent film having irregularities on the fiber base material, and it has succeeded in imparting high water repellency. However, it is necessary to use a large amount of organic solvent in order to disperse the hydrophobic particles in the processing liquid, which is not desirable from the viewpoint of reducing the environmental load.
Further, none of the above-mentioned patent documents discloses specific technical means for improving washing durability.
以上の従来技術に鑑み、本発明が解決しようとする課題は、高い撥水性と洗濯耐久性を有する撥水性布帛、並びに有機溶媒の使用を低減した該撥水性布帛の製造方法を提供することである。 In view of the above prior art, the problem to be solved by the present invention is to provide a water-repellent fabric having high water repellency and washing durability, and a method for producing the water-repellent fabric with reduced use of an organic solvent. is there.
本願発明者は、前記課題を解決すべく鋭意研究し実験を重ねた結果、布帛を構成する繊維の表面に、所定粒子径の親水性粒子と、該親水性粒子を覆う撥水剤及びバインダー樹脂とから構成される被膜を形成することで、前記課題を解決できることを予想外に見出し、本発明を完成するに至ったものである。 As a result of diligent research and experiments to solve the above problems, the inventor of the present application has hydrophilic particles having a predetermined particle size on the surface of the fibers constituting the fabric, and a water repellent and a binder resin covering the hydrophilic particles. It was unexpectedly found that the above-mentioned problems could be solved by forming a film composed of and, and the present invention was completed.
すなわち、本発明は以下の通りのものである。
［１］繊維表面に、平均一次粒子径が４０ｎｍ〜６００ｎｍである親水性粒子と、該親水性粒子を覆う撥水剤及びバインダー樹脂とから構成される被膜を有する繊維から構成される撥水性布帛。
［２］前記被膜が、親水性粒子を覆うバインダー樹脂層と、該バインダー樹脂層を覆う撥水剤及びバインダー樹脂からなる層とからなる２層構造を有する、前記［１］に記載の撥水性布帛。
［３］前記被膜中の撥水剤が、フッ素共重合物、長鎖アルキル共重合物、及びシリコーン共重合物からなる群から選択される少なくとも１種である、前記［１］又は［２］に記載の撥水性布帛。
［４］前記親水性粒子が、ラテックス、アルミニウム化合物、ケイ素化合物、及びチタン化合物からなる群から選択される少なくとも１種である、前記［１］〜［３］のいずれかに記載の撥水性布帛。
［５］前記バインダー樹脂が、ブロックドイソシアネート又はＮ−メチロールメラミンの反応生成物である、前記［１］〜［４］のいずれかに記載の撥水性布帛。
［６］以下の工程：
親水性粒子、バインダー樹脂原料、及び撥水剤を含む水分散体に布帛を浸漬した後に乾燥させる工程；
を少なくとも１回含む、前記［１］、及び［３］〜［５］のいずれかに記載の撥水性布帛の製造方法。
［７］以下の工程：
親水性粒子、及びバインダー樹脂原料を含む水分散体に布帛を浸漬した後に乾燥させる工程；
得られた布帛を、バインダー樹脂原料、及び撥水剤を含む水分散体に浸漬した後に乾燥させる工程；
を、それぞれ、少なくとも１回含む、前記［２］〜［６］のいずれかに記載の撥水性布帛の製造方法。
［８］前記バインダー樹脂原料が、ブロックドイソシアネート又はＮ−メチロールメラミンである、前記［６］又は［７］に記載の方法。
That is, the present invention is as follows.
[1] A water-repellent fabric composed of fibers having a film on the fiber surface, which is composed of hydrophilic particles having an average primary particle diameter of 40 nm to 600 nm and a water-repellent agent and a binder resin covering the hydrophilic particles. ..
[2] The water repellency according to the above [1], wherein the coating film has a two-layer structure including a binder resin layer covering hydrophilic particles and a layer made of a water repellent agent and a binder resin covering the binder resin layer. Fabric.
[3] The water repellent in the coating is at least one selected from the group consisting of a fluorine copolymer, a long-chain alkyl copolymer, and a silicone copolymer, according to the above [1] or [2]. The water-repellent fabric according to.
[4] The water-repellent fabric according to any one of [1] to [3] above, wherein the hydrophilic particles are at least one selected from the group consisting of latex, aluminum compounds, silicon compounds, and titanium compounds. ..
[5] The water-repellent fabric according to any one of [1] to [4] above, wherein the binder resin is a reaction product of blocked isocyanate or N-methylol melamine.
[6] The following steps:
A step of immersing the fabric in an aqueous dispersion containing hydrophilic particles, a binder resin raw material, and a water repellent, and then drying the fabric;
The method for producing a water-repellent fabric according to any one of [1] and [3] to [5] above, which comprises at least once.
[7] The following steps:
A step of immersing the fabric in an aqueous dispersion containing hydrophilic particles and a binder resin raw material and then drying the fabric;
A step of immersing the obtained fabric in an aqueous dispersion containing a binder resin raw material and a water repellent and then drying the fabric;
The method for producing a water-repellent fabric according to any one of the above [2] to [6], which comprises at least once, respectively.
[8] The method according to [6] or [7] above, wherein the binder resin raw material is blocked isocyanate or N-methylol melamine.
本発明に係る撥水性布帛は、布帛を構成する繊維（糸）の表面に適切な凹凸形状を有する撥水性被膜が形成されているため、高い撥水性と洗濯耐久性を有する布帛となる。また、該布帛の製造プロセスは、有機溶媒の使用量を低減したものとなる。それゆえ、本発明は、防汚・防水の観点から、良好かつ洗濯耐久性を有する撥水性を備えた布帛、例えば、レインコートやダウンジャケットなどのアパレル製品として、またその製造方法として好適に利用可能である。 The water-repellent fabric according to the present invention is a fabric having high water repellency and washing durability because a water-repellent film having an appropriate uneven shape is formed on the surface of the fibers (threads) constituting the fabric. In addition, the fabric manufacturing process reduces the amount of organic solvent used. Therefore, from the viewpoint of antifouling and waterproofing, the present invention is suitably used as a water-repellent fabric having good and washing durability, for example, as an apparel product such as a raincoat or a down jacket, and as a manufacturing method thereof. It is possible.
以下、本発明の実施形態を詳細に説明する。
本実施形態の撥水性布帛は、繊維表面に、平均一次粒子径が４０ｎｍ〜６００ｎｍである親水性粒子と、該親水性粒子を覆う撥水剤及びバインダー樹脂とから構成される被膜を有する繊維から構成されるものであることを特徴とする。
本実施形態の撥水性布帛における繊維表面に存在する被膜表面の拡大写真を図１に示す。尚、本発明は図１に示すものに限定されるものではない。
Hereinafter, embodiments of the present invention will be described in detail.
The water-repellent fabric of the present embodiment is made of a fiber having a film on the fiber surface composed of hydrophilic particles having an average primary particle diameter of 40 nm to 600 nm and a water-repellent agent and a binder resin covering the hydrophilic particles. It is characterized in that it is composed.
FIG. 1 shows an enlarged photograph of the coating surface existing on the fiber surface in the water-repellent fabric of the present embodiment. The present invention is not limited to that shown in FIG.
図１に示すように、撥水性布帛１は、布帛を構成する繊維２、及び繊維２の表面に形成された被膜３からなる。被膜３は、親水性粒子４と、これを覆う撥水剤５とバインダー樹脂６の混合物から構成される。尚、撥水剤５とバインダー樹脂６の混合物が親水性粒子４を全て覆うことが望ましいが、覆われていない部分が僅かに存在していたとしても構わない。被膜３の表面には、親水性粒子５の立体構造に起因する凹凸形状が形成されため、布帛を構成する繊維２の表面上に緻密な凹凸を有する撥水性被膜が形成され、蓮の葉効果が発現することで、高い撥水性が発現する。尚、被膜３は繊維２の表面全てを被覆していることが望ましいが、局所的に被膜が形成されていない部分がある場合にも高い撥水性が発現する。
As shown in FIG. 1, the water-repellent fabric 1 is composed of
親水性粒子４としては、親水性を有するものであれば特に限定されないが、アルミニウム酸化物、ケイ素酸化物、チタン酸化物などの無機酸化物粒子、ラテックス、アクリル、ナイロンなどの有機物粒子が例として挙げられる。これらの内、取り扱いが容易であることから、特に、ケイ素酸化物粒子、チタン酸化物粒子、アルミニウム酸化物粒子が好ましい。これらの市販品として、ケイ素酸化物粒子としては、「スノーテックスＳＴ−ＯＹＬ」、「スノーテックスＳＴ−ＡＫ−Ｌ」および「スノーテックスＳＴ−ＡＫ−ＹＬ」（以上、日産化学株式会社製）、チタン酸化物粒子としては、「ＴＡ３００」および「ＴＡ３００Ｄ」（以上、富士チタン工業株式会社製）、アルミニウム酸化物粒子としては、「ＴＭ−５Ｄ」（大明化学工業株式会社製）が例示できる。
尚、ここでいう親水性とは、粒子が水溶媒に対して容易に分散する性質のことである。具体的には、水溶媒に対して粒子粉末を１．０質量％および任意の分散剤を添加し、ホモミキサーを用いて７００ｒｐｍで１０分攪拌した後、１時間静置した場合に、目視により粒子の沈殿又は凝集が確認できない場合には親水性を有していることとする。また、粒子を水溶媒に分散させた状態で市販されている粒子水分散体についても、含有されている粒子は親水性を有していることとする。
The hydrophilic particles 4 are not particularly limited as long as they have hydrophilicity, but examples thereof include inorganic oxide particles such as aluminum oxide, silicon oxide and titanium oxide, and organic particles such as latex, acrylic and nylon. Can be mentioned. Of these, silicon oxide particles, titanium oxide particles, and aluminum oxide particles are particularly preferable because they are easy to handle. As these commercially available products, as silicon oxide particles, "Snowtex ST-OYL", "Snowtex ST-AK-L" and "Snowtex ST-AK-YL" (all manufactured by Nissan Chemicals Co., Ltd.), Examples of the titanium oxide particles include "TA300" and "TA300D" (manufactured by Fuji Titanium Industry Co., Ltd.), and examples of the aluminum oxide particles include "TM-5D" (manufactured by Taimei Chemicals Co., Ltd.).
The term "hydrophilicity" as used herein means that the particles are easily dispersed in an aqueous solvent. Specifically, when 1.0% by mass of the particle powder and an arbitrary dispersant were added to the aqueous solvent, the mixture was stirred at 700 rpm for 10 minutes using a homomixer, and then allowed to stand for 1 hour, visually. If the precipitation or aggregation of particles cannot be confirmed, it is considered to be hydrophilic. Further, it is also assumed that the contained particles of the particle aqueous dispersion, which is commercially available in the state where the particles are dispersed in an aqueous solvent, have hydrophilicity.
親水性粒子４の平均一次粒子径としては、４０ｎｍ〜６００ｎｍであればよいが、より高い撥水性を発現させるためには、４０ｎｍ〜４００ｎｍが好ましく、６０ｎｍ〜２００ｎｍがより好ましい。平均一次粒子径が４０ｎｍ未満であると、接触角が低下する。他方、平均一次粒子径が６００ｎｍを超えると、被膜の透明性がなくなり、生地の外観を損ねる。
平均一次粒子径は走査型電子顕微鏡（ＦＥ−ＳＥＭ）で測定することができる。具体的には、まず、ＦＥ−ＳＥＭにより生地の任意の位置を任意の倍率により上方から観察する。次に、粒子形状が球状の場合には、その直径、非球状の場合には、最長径と最短径の平均値を粒子径（粒径）と見なすこととする。視野内に存在する全ての粒子の粒径を測定し、視野を移動して再度粒径を測定することを繰り返すことで、粒径を１０点以上測定し、その平均値を平均一次粒子径とする。
The average primary particle diameter of the hydrophilic particles 4 may be 40 nm to 600 nm, but in order to develop higher water repellency, 40 nm to 400 nm is preferable, and 60 nm to 200 nm is more preferable. If the average primary particle size is less than 40 nm, the contact angle decreases. On the other hand, if the average primary particle size exceeds 600 nm, the transparency of the coating is lost and the appearance of the fabric is impaired.
The average primary particle size can be measured with a scanning electron microscope (FE-SEM). Specifically, first, an arbitrary position of the dough is observed from above at an arbitrary magnification by FE-SEM. Next, when the particle shape is spherical, its diameter is regarded as its diameter, and when it is non-spherical, the average value of the longest diameter and the shortest diameter is regarded as the particle diameter (particle size). By measuring the particle size of all the particles existing in the field of view, moving the field of view, and repeating the measurement of the particle size again, the particle size is measured at 10 points or more, and the average value is taken as the average primary particle size. To do.
撥水剤５としては、繊維表面に疎水性の被膜を形成することが可能であるものであれば特に制限されず、例えば、フッ素系撥水剤、長鎖アルキル系撥水剤、シリコーン系撥水剤、アクリル系撥水剤、ウレタン系撥水剤、パラフィンワックス等が挙げられる。これらの内、フッ素共重合物、長鎖アルキル共重合物、シリコーン共重合物からなる群から選択される少なくとも１つ以上を主成分とする撥水剤が望ましい。これらの市販品として、フッ素共重合物を主成分とする撥水剤としては、「ＡｓａｈｉＧｕａｒｄ Ｅ−ＳＥＲＩＥＳ ＡＧ−Ｅ０８２」（明成化学工業株式会社製）、長鎖アルキル共重合物を主成分とする撥水剤としては、「メイシールドＺ−１」、「メイシールドＰ−３５０Ｋ」（以上、明成化学工業株式会社製）、「ネオシードＮＲ−７０８０」、「ネオシードＮＲ−７２００」（以上、日華化学株式会社製）、シリコーン共重合物を主成分とする撥水剤としては、「ネオシードＮＲ−８０００」（日華化学株式会社製）が例示できる。尚、複数種類の撥水剤を混合したものを用いてもよい。 The water repellent 5 is not particularly limited as long as it can form a hydrophobic film on the fiber surface. For example, a fluorine-based water repellent, a long-chain alkyl-based water repellent, and a silicone-based water repellent. Examples thereof include water agents, acrylic water repellents, urethane water repellents, paraffin wax and the like. Of these, a water repellent containing at least one selected from the group consisting of a fluorine copolymer, a long-chain alkyl copolymer, and a silicone copolymer as a main component is desirable. As these commercially available products, as a water repellent containing a fluorine copolymer as a main component, "AsahiGuard E-SERIES AG-E082" (manufactured by Meisei Chemical Works, Ltd.), a long-chain alkyl copolymer as a main component is used. As water repellents, "Mayshield Z-1", "Mayshield P-350K" (above, manufactured by Meisei Chemical Works, Ltd.), "Neoseed NR-7080", "Neoseed NR-7200" (above, Nicca) As a water repellent agent containing a silicone copolymer as a main component (manufactured by Chemical Co., Ltd.), “Neoseed NR-8000” (manufactured by Nicca Chemical Works, Ltd.) can be exemplified. A mixture of a plurality of types of water repellents may be used.
バインダー樹脂６とは、被膜内で化学的に架橋構造を形成することより、繊維表面と、親水性粒子及び撥水剤とを物理的に接続する役割を有する樹脂であり、被膜に物理的耐久性を付与する効果がある。化学反応によりバインダー樹脂を形成するバインダー樹脂原料としては、前記役割を果たす架橋剤であれば特に制限されないが、環境負荷低減のために有機溶剤の使用量が少ない架橋剤が好ましく、水系エマルジョン化された架橋剤が量産化されている、ブロックドイソシアネート又はＮ−メチロールメラミンが好ましい。これらの市販品としては、「メイカネートＦＭ−１」、「メイカネートＰＲＯ」、「メイカネートＣＸ」、「ＳＵ−２６８」（以上、明成化学工業株式会社製）、「ＮＫアシストＦＵ」、「ＵＮＩＫＡＲＥＳＩＮ ３８０−Ｋ」（以上、日華化学株式会社製）が挙げられる。 The binder resin 6 is a resin having a role of physically connecting the fiber surface with hydrophilic particles and a water repellent by chemically forming a crosslinked structure in the coating film, and is physically durable to the coating film. It has the effect of imparting sex. The binder resin raw material for forming the binder resin by a chemical reaction is not particularly limited as long as it is a cross-linking agent that plays the above-mentioned role. However, in order to reduce the environmental load, a cross-linking agent that uses a small amount of organic solvent is preferable, and an aqueous emulsion is formed. Blocked isocyanate or N-methylol melamine, which has been mass-produced as a cross-linking agent, is preferable. These commercially available products include "Meikanate FM-1", "Meikanate PRO", "Meikanate CX", "SU-268" (manufactured by Meisei Chemical Works, Ltd.), "NK Assist FU", and "UNIKARESIN 380-". K ”(above, manufactured by Nicca Chemical Works, Ltd.) can be mentioned.
被膜３は、図２に示すように、親水性粒子と、該親水性粒子を覆う撥水剤及びバインダー樹脂とから構成される単一の層であることができる。この態様の場合には、以下の工程：
親水性粒子、バインダー樹脂原料、及び撥水剤を含む水分散体に布帛を浸漬した後に乾燥させる工程；
を少なくとも１回含む方法により、かかる被膜が繊維表面に形成された撥水性布帛を製造することができる。
As shown in FIG. 2, the
A step of immersing the fabric in an aqueous dispersion containing hydrophilic particles, a binder resin raw material, and a water repellent, and then drying the fabric;
A water-repellent fabric having such a coating formed on the fiber surface can be produced by a method containing at least once.
あるいは、被膜３は、図３に示すように、親水性粒子を覆うバインダー樹脂層と、該バインダー樹脂層を覆う撥水剤及びバインダー樹脂からなる層とからなる２層構造を有するものであることができる。この態様の場合には、以下の工程：
親水性粒子、及びバインダー樹脂原料を含む水分散体に布帛を浸漬した後に乾燥させる工程；
得られた布帛を、バインダー樹脂原料、及び撥水剤を含む水分散体に浸漬した後に乾燥させる工程；
を、それぞれ、少なくとも１回含む方法により、かかる被膜が繊維表面に形成された撥水性布帛を製造することができる。かかる製造方法は、親水性粒子と撥水剤とを混合することがない、例えば、親水性粒子と撥水剤の相溶性が悪く混合できない場合や、粒子と撥水剤の混合により凝集体を生じる場合であっても、撥水性被膜を形成できる点で、好ましい。
Alternatively, as shown in FIG. 3, the
A step of immersing the fabric in an aqueous dispersion containing hydrophilic particles and a binder resin raw material and then drying the fabric;
A step of immersing the obtained fabric in an aqueous dispersion containing a binder resin raw material and a water repellent and then drying the fabric;
A water-repellent fabric having such a coating formed on the fiber surface can be produced by a method containing each of the above at least once. Such a production method does not mix the hydrophilic particles and the water repellent, for example, when the hydrophilic particles and the water repellent are poorly compatible and cannot be mixed, or when the particles and the water repellent are mixed to form an agglomerate. Even if it occurs, it is preferable in that a water-repellent film can be formed.
尚、被膜３は、撥水剤、バインダー樹脂、及び親水性粒子に加えて、所望の効果を損なわない限り、任意の添加剤を含んでもよい。添加剤としては、例えば、防しわ剤、難燃剤、帯電防止剤、耐熱剤等の繊維用薬剤、酸化防止剤、紫外線吸収剤、顔料、硬化促進剤、消臭剤、抗菌剤等が挙げられる。これらの添加剤は複数種類を組み合わせて用いてもよい。
In addition to the water repellent, the binder resin, and the hydrophilic particles, the
本実施形態の撥水性布帛を構成する撥水処理が施される繊維の種類は、所望の効果を生じる限り特に制限されず、ナイロン、ポリエステル、アクリル、ポリウレタン等の合成繊維、綿、麻、絹、ウール等の天然繊維、これらを組み合わせた繊維を挙げることができる。また、本実施形態の撥水性布帛は、繊維から構成されるものである限り、特に制限はないが、編物、織物、不織布等を挙げることができる。尚、本発明においては、ナイロン薄地織物において特に優れた撥水性を発現させることができる。 The type of fiber to which the water-repellent treatment is applied constituting the water-repellent fabric of the present embodiment is not particularly limited as long as the desired effect is produced, and synthetic fibers such as nylon, polyester, acrylic and polyurethane, cotton, linen and silk. , Natural fibers such as wool, and fibers that combine these. The water-repellent fabric of the present embodiment is not particularly limited as long as it is composed of fibers, and examples thereof include knitted fabrics, woven fabrics, and non-woven fabrics. In the present invention, particularly excellent water repellency can be exhibited in a nylon thin woven fabric.
以下、実施例、比較例を挙げて本発明を具体的に説明するが、本発明は実施例に何ら限定されるものではない。実施例及び比較例に用いた各種特性の評価方法は以下の通りであった。 Hereinafter, the present invention will be specifically described with reference to Examples and Comparative Examples, but the present invention is not limited to the Examples. The evaluation methods of various characteristics used in Examples and Comparative Examples were as follows.
＜撥水性（接触角の測定）＞
実施例１〜１５、及び比較例１〜９で得た撥水性布帛の接触角を測定した。測定には全自動接触角計測装置（協和科学製ＦＡＣＥ）を用いた。試験片は布帛から１ｃｍ×１ｃｍの大きさの布帛３枚をランダムに切り出したものとした。試験片の中心に蒸留水３５μｍを滴下し、１．０秒後の画像を取得した後、該接触角計の自動フィッティング機能を用いて接触角を測定した。接触角が大きいほど、撥水性が高いことを示す。
<Water repellency (measurement of contact angle)>
The contact angles of the water-repellent fabrics obtained in Examples 1 to 15 and Comparative Examples 1 to 9 were measured. A fully automatic contact angle measuring device (FACE manufactured by Kyowa Kagaku) was used for the measurement. As the test piece, three pieces of cloth having a size of 1 cm × 1 cm were randomly cut out from the cloth. After dropping 35 μm of distilled water onto the center of the test piece and acquiring an image 1.0 second later, the contact angle was measured using the automatic fitting function of the contact angle meter. The larger the contact angle, the higher the water repellency.
＜洗濯耐久性＞
実施例１〜１５、及び比較例１〜９で得た撥水性布帛の撥水度の洗濯耐久性を測定した。作製した撥水性布帛を洗濯回数０回（ＨＬ−０）とし、ＪＩＳ Ｌ １０９２（２００９）に記載の洗濯方法に則り、洗濯を２０回（ＨＬ−２０）行い、自然乾燥を行った後、ＪＩＳ Ｌ １０９２（２００９）のスプレー法にて撥水度を評価した。尚、撥水度評価は、以下に示す１〜５の５段階の数値にて表記した。
５：表面に湿潤及び水滴の付着がない。
４：表面に湿潤しないが、小さな水滴の付着を示す。
３：表面に小さな個々の水滴状の湿潤を示す。
２：表面の半分に湿潤を示し、小さな個々の湿潤が布の表面を浸透する状態を示す。
１：表面全体に湿潤を示す。
５が最も撥水度が高く、ＨＬ−２０の撥水度が高いものほど、洗濯耐久性が高い。
<Washing durability>
The washing durability of the water repellency of the water repellent fabrics obtained in Examples 1 to 15 and Comparative Examples 1 to 9 was measured. The produced water-repellent fabric was washed 0 times (HL-0), washed 20 times (HL-20) according to the washing method described in JIS L 1092 (2009), air-dried, and then JIS. The water repellency was evaluated by the spray method of L 1092 (2009). The water repellency evaluation was expressed by a numerical value of 5 levels from 1 to 5 shown below.
5: No wetting or water droplets adhering to the surface.
4: Does not wet the surface, but shows the adhesion of small water droplets.
3: Shows small individual water droplet-like wetness on the surface.
2: Wetness is shown on half of the surface, and small individual wettings penetrate the surface of the cloth.
1: Shows wetness on the entire surface.
5 has the highest water repellency, and the higher the water repellency of HL-20, the higher the washing durability.
［実施例１］
ナイロン６仮撚加工糸からなる織物を基材とし、フッ素系共重合物を主成分とする撥水剤（ＡｓａｈｉＧｕａｒｄ Ｅ−ＳＥＲＩＥＳ ＡＧ−Ｅ０８２（明成化学工業株式会社製））５部、ケイ素化合物とアルミニウム化合物の複合物を主成分とする平均一次粒子径４０ｎｍの親水性粒子（スノーテックスＳＴ−ＡＫ−Ｌ（日産化学株式会社製））０．５部、並びにブロックドイソシアネートを主成分とするバインダー樹脂（メイカネートＦＭ―１（明成化学工業株式会社製））１部の混合水分散体を、基材にパディングし、２本のゴムローラーでニップ（ピックアップ率６７％）し、１００℃にて９０秒間乾燥させた後、１８０℃にて９０秒間キュアを行うことにより、撥水性布帛を作製した。
[Example 1]
5 parts of water repellent (AsahiGuard E-SERIES AG-E082 (manufactured by Meisei Chemical Works, Ltd.)) whose base material is a woven fabric made of nylon 6 false twisted yarn and whose main component is a fluorine-based copolymer, and a silicon compound. 0.5 parts of hydrophilic particles (Snowtex ST-AK-L (manufactured by Nissan Chemical Co., Ltd.)) with an average primary particle diameter of 40 nm containing a composite of aluminum compounds as the main component, and a binder containing blocked isocyanate as the main component. A mixed aqueous dispersion of 1 part of a resin (Makenate FM-1 (manufactured by Meisei Chemical Works, Ltd.)) was padded on a base material, nipped with two rubber rollers (pickup rate 67%), and 90 at 100 ° C. A water-repellent cloth was prepared by drying for seconds and then curing at 180 ° C. for 90 seconds.
［実施例２］
ナイロン６仮撚加工糸からなる織物を基材とし、フッ素系共重合物を主成分とする撥水剤（ＡｓａｈｉＧｕａｒｄ Ｅ−ＳＥＲＩＥＳ ＡＧ−Ｅ０８２（明成化学工業株式会社製））５部、ケイ素化合物とアルミニウム化合物の複合物を主成分とする平均一次粒子径１１０ｎｍの親水性粒子（スノーテックスＳＴ−ＡＫ−ＹＬ（日産化学株式会社製））０．５部、並びにブロックドイソシアネートを主成分とするバインダー樹脂の混合水分散体（メイカネートＦＭ―１（明成化学工業株式会社製））１部を、実施例１と同様に基材に加工することにより、撥水性布帛を作製した。
[Example 2]
5 parts of water repellent (AsahiGuard E-SERIES AG-E082 (manufactured by Meisei Chemical Works, Ltd.)) whose base material is a woven fabric made of nylon 6 false twisted yarn and whose main component is a fluorine-based copolymer, and a silicon compound. 0.5 parts of hydrophilic particles (Snowtex ST-AK-YL (manufactured by Nissan Chemical Co., Ltd.)) with an average primary particle diameter of 110 nm containing a composite of aluminum compounds as the main component, and a binder containing blocked isocyanate as the main component. A water-repellent cloth was prepared by processing one part of a mixed aqueous dispersion of resin (Meicanate FM-1 (manufactured by Meisei Chemical Works, Ltd.)) into a base material in the same manner as in Example 1.
［実施例３］
ナイロン６仮撚加工糸からなる織物を基材とし、長鎖アルキル共重合物を主成分とする撥水剤（メイシールドＺ−１（明成化学工業株式会社製））５部、ケイ素化合物とアルミニウム化合物の複合物を主成分とする平均一次粒子径１１０ｎｍの親水性粒子（スノーテックスＳＴ−ＡＫ−ＹＬ（日産化学株式会社製））０．５部、並びにブロックドイソシアネートを主成分とするバインダー樹脂の混合水分散体（メイカネートＦＭ―１（明成化学工業株式会社製））１部を、実施例１と同様に基材に加工することにより、撥水性布帛を作製した。
[Example 3]
5 parts of water repellent (Mayshield Z-1 (manufactured by Meisei Chemical Works, Ltd.)) whose base material is a woven fabric made of nylon 6 false twisted yarn and whose main component is a long-chain alkyl copolymer, silicon compound and aluminum. 0.5 parts of hydrophilic particles (Snowtex ST-AK-YL (manufactured by Nissan Chemical Co., Ltd.)) having an average primary particle diameter of 110 nm containing a composite of compounds as the main component, and a binder resin containing blocked isocyanate as the main component. A water-repellent cloth was prepared by processing one part of the mixed aqueous dispersion (Meikanate FM-1 (manufactured by Meisei Chemical Works, Ltd.)) into a base material in the same manner as in Example 1.
［実施例４］
ナイロン６仮撚加工糸からなる織物を基材とし、長鎖アルキル共重合物を主成分とする撥水剤（ネオシードＮＲ７２００（日華化学株式会社製））５部、ケイ素化合物とアルミニウム化合物の複合物を主成分とする平均一次粒子径１１０ｎｍの親水性粒子（スノーテックスＳＴ−ＡＫ−ＹＬ（日産化学株式会社製））０．５部、並びにＮ−メチロールメラミンを主成分とするバインダー樹脂の混合水分散体（ＵＮＩＫＡＲＥＳＩＮ ３８０−Ｋ（日華化学株式会社製））１部を、実施例１と同様に基材に加工することにより、撥水性布帛を作製した。
[Example 4]
5 parts of water repellent (Neoseed NR7200 (manufactured by Nicca Chemical Co., Ltd.)) whose base material is a woven fabric made of nylon 6 false twisted yarn and whose main component is a long-chain alkyl copolymer, and a composite of a silicon compound and an aluminum compound. A mixture of 0.5 parts of hydrophilic particles (Snowtex ST-AK-YL (manufactured by Nicca Chemical Co., Ltd.)) having an average primary particle diameter of 110 nm and a binder resin containing N-methylol melamine as the main component. A water-repellent cloth was prepared by processing one part of an aqueous dispersion (UNIKARESIN 380-K (manufactured by Nicca Chemical Co., Ltd.)) into a base material in the same manner as in Example 1.
［実施例５］
ナイロン６仮撚加工糸からなる織物を基材とし、シリコーン系共重合物を主成分とする撥水剤（ネオシードＮＲ８０００（日華化学株式会社製））５部、ケイ素化合物とアルミニウム化合物の複合物を主成分とする平均一次粒子径１１０ｎｍの親水性粒子（スノーテックスＳＴ−ＡＫ−ＹＬ（日産化学株式会社製））０．５部、並びにブロックドイソシアネートを主成分とするバインダー樹脂の混合水分散体（ＮＫアシストＦＵ（日華化学株式会社製））１部を、実施例１と同様に基材に加工することにより、撥水性布帛を作製した。
[Example 5]
5 parts of water repellent (Neoseed NR8000 (manufactured by Nicca Chemical Co., Ltd.)) whose base material is a woven fabric made of nylon 6 false twisted yarn and whose main component is a silicone copolymer, and a composite of a silicon compound and an aluminum compound 0.5 parts of hydrophilic particles (Snowtex ST-AK-YL (manufactured by Nicca Chemical Co., Ltd.)) having an average primary particle diameter of 110 nm, and a mixed aqueous dispersion of a binder resin containing blocked isocyanate as the main component. A water-repellent cloth was produced by processing one part of a body (NK Assist FU (manufactured by Nicca Chemical Co., Ltd.)) into a base material in the same manner as in Example 1.
［実施例６］
ナイロン６仮撚加工糸からなる織物を基材とし、シリコーン系共重合物を主成分とする撥水剤（ネオシードＮＲ８０００（日華化学株式会社製））２．５部と長鎖アルキル共重合物を主成分とする撥水剤（ネオシードＮＲ７２００（日華化学株式会社製））２．５部を混合した撥水剤、ケイ素化合物とアルミニウム化合物の複合物を主成分とする平均一次粒子径１１０ｎｍの親水性粒子（スノーテックスＳＴ−ＡＫ−ＹＬ（日産化学株式会社製））０．５部、並びにブロックドイソシアネートを主成分とするバインダー樹脂（ＮＫアシストＦＵ（日華化学株式会社製））１部の混合水分散体を、実施例１と同様に基材に加工することにより、撥水性布帛を作製した。
[Example 6]
2.5 parts of a water repellent (Neoseed NR8000 (manufactured by Nicca Chemical Co., Ltd.)) whose base material is a woven fabric made of nylon 6 false twisted yarn and whose main component is a silicone-based copolymer and a long-chain alkyl copolymer. Water repellent containing 2.5 parts of a water repellent containing 2.5 parts (Neoseed NR7200 (manufactured by Nicca Chemical Co., Ltd.)), an average primary particle diameter of 110 nm containing a composite of a silicon compound and an aluminum compound as the main component. 0.5 parts of hydrophilic particles (Snowtex ST-AK-YL (manufactured by Nicca Chemical Co., Ltd.)) and 1 part of binder resin containing blocked isocyanate as the main component (NK Assist FU (manufactured by Nicca Chemical Co., Ltd.)) A water-repellent cloth was prepared by processing the mixed aqueous dispersion of No. 1 into a base material in the same manner as in Example 1.
［実施例７］
ナイロン６仮撚加工糸からなる織物を基材とし、フッ素系共重合物を主成分とする撥水剤（ＡｓａｈｉＧｕａｒｄ Ｅ−ＳＥＲＩＥＳ ＡＧ−Ｅ０８２（明成化学工業株式会社製））５部、アルミニウム化合物の複合物を主成分とする平均一次粒子径２００ｎｍの親水性粒子（ＴＭ−５Ｄ（大明化学工業株式会社））０．５部、並びにブロックドイソシアネートを主成分とするバインダー樹脂（メイカネートＦＭ―１（明成化学工業株式会社製））１部の混合水分散体を、実施例１と同様に基材に加工することにより、撥水性布帛を作製した。
[Example 7]
5 parts of water repellent (AsahiGuard E-SERIES AG-E082 (manufactured by Meisei Chemical Works, Ltd.)) whose base material is a woven fabric made of nylon 6 false twisted yarn and whose main component is a fluorine-based copolymer, and an aluminum compound. 0.5 parts of hydrophilic particles (TM-5D (Taimei Chemicals Co., Ltd.)) having an average primary particle diameter of 200 nm containing a composite as a main component, and a binder resin containing blocked isocyanate as a main component (Meicanate FM-1 (Meisei FM-1)). (Made by Meisei Chemical Works, Ltd.)) A water-repellent cloth was prepared by processing a part of the mixed aqueous dispersion into a base material in the same manner as in Example 1.
［実施例８］
ナイロン６仮撚加工糸からなる織物を基材とし、フッ素系共重合物を主成分とする撥水剤（ＡｓａｈｉＧｕａｒｄ Ｅ−ＳＥＲＩＥＳ ＡＧ−Ｅ０８２（明成化学工業株式会社製））５部、チタン化合物の複合物を主成分とする平均一次粒子径４００ｎｍの親水性粒子（ＴＡ３００Ｄ（富士チタン工業株式会社製））０．５部、並びにブロックドイソシアネートを主成分とするバインダー樹脂（メイカネートＦＭ―１（明成化学工業株式会社製））１部の混合水分散体を、実施例１と同様に基材に加工することにより、撥水性布帛を作製した。
[Example 8]
5 parts of water repellent (AsahiGuard E-SERIES AG-E082 (manufactured by Meisei Chemical Works, Ltd.)) based on a woven fabric made of nylon 6 false twisted yarn and containing a fluorine-based copolymer as a main component, and a titanium compound. 0.5 parts of hydrophilic particles (TA300D (manufactured by Fuji Titanium Industry Co., Ltd.)) with an average primary particle diameter of 400 nm containing the composite as the main component, and a binder resin (Meisei FM-1 (Meisei)) containing blocked isocyanate as the main component. (Manufactured by Kagaku Kogyo Co., Ltd.)) A water-repellent cloth was produced by processing a part of the mixed aqueous dispersion into a base material in the same manner as in Example 1.
［実施例９］
ナイロン６仮撚加工糸からなる織物を基材とし、フッ素系共重合物を主成分とする撥水剤（ＡｓａｈｉＧｕａｒｄ Ｅ−ＳＥＲＩＥＳ ＡＧ−Ｅ０８２（明成化学工業株式会社製））５部、チタン化合物の複合物を主成分とする平均一次粒子径６００ｎｍの親水性粒子（ＴＡ３００（富士チタン工業株式会社製））０．５部、並びにブロックドイソシアネートを主成分とするバインダー樹脂（メイカネートＦＭ―１（明成化学工業株式会社製））１部の混合水分散体を、実施例１と同様に基材に加工することにより、撥水性布帛を作製した。
[Example 9]
5 parts of water repellent (AsahiGuard E-SERIES AG-E082 (manufactured by Meisei Chemical Works, Ltd.)) based on a woven fabric made of nylon 6 false twisted yarn and containing a fluorine-based copolymer as a main component, and a titanium compound. 0.5 parts of hydrophilic particles (TA300 (manufactured by Fuji Titanium Industry Co., Ltd.)) having an average primary particle diameter of 600 nm containing a composite as a main component, and a binder resin containing blocked isocyanate as a main component (Meisei FM-1 (Meisei Chemical Works)). (Manufactured by Kagaku Kogyo Co., Ltd.)) A water-repellent cloth was produced by processing a part of the mixed aqueous dispersion into a base material in the same manner as in Example 1.
［実施例１０］
ナイロン６仮撚加工糸からなる織物を基材とし、ラテックスを主成分とする平均一次粒子径８０ｎｍの親水性粒子（ＰＶコート剤（旭化成株式会社製））０．５％、及びブロックドイソシアネートを主成分とするバインダー樹脂（ＳＵ−２６８（明成化学工業株式会社製））１部の混合水分散体を、基材に浸漬した後に乾燥させ、次いで、フッ素系共重合物を主成分とする撥水剤（ＡｓａｈｉＧｕａｒｄ Ｅ−ＳＥＲＩＥＳ ＡＧ−Ｅ０８２（明成化学工業株式会社製））５部とブロックドイソシアネートを主成分とするバインダー樹脂（メイカネートＦＭ―１（明成化学工業株式会社製））１部との混合水分散体を、実施例１と同様に基材に加工することにより、撥水性布帛を作製した。
[Example 10]
Using a woven fabric made of nylon 6 false twisted yarn as a base material, 0.5% of hydrophilic particles (PV coating agent (manufactured by Asahi Kasei Co., Ltd.)) containing latex as the main component and an average primary particle diameter of 80 nm, and blocked isocyanate. A mixed aqueous dispersion of a part of a binder resin (SU-268 (manufactured by Meisei Chemical Works, Ltd.)) as a main component is dipped in a base material and then dried, and then repellent containing a fluorine-based copolymer as a main component. 5 parts of liquid agent (AsahiGuard E-SERIES AG-E082 (manufactured by Meisei Chemical Works, Ltd.)) and 1 part of binder resin (polymer FM-1 (manufactured by Meisei Chemical Works, Ltd.)) containing blocked isocyanate as a main component. A water-repellent cloth was prepared by processing the mixed aqueous dispersion into a base material in the same manner as in Example 1.
［実施例１１］
ナイロン６仮撚加工糸からなる織物を基材とし、ケイ素化合物を主成分とする平均一次粒子径６０ｎｍの親水性粒子（スノーテックスＳＴ−ＯＹＬ（日産化学製））、及びブロックドイソシアネートを主成分とするバインダー樹脂の混合水分散体（ＳＵ−２６８（明成化学工業株式会社製））１部を、基材に浸漬した後に乾燥させ、次いで、フッ素系共重合物を主成分とする撥水剤（ＡｓａｈｉＧｕａｒｄ Ｅ−ＳＥＲＩＥＳ ＡＧ−Ｅ０８２（明成化学工業株式会社製））５部とブロックドイソシアネートを主成分とするバインダー樹脂（メイカネートＦＭ―１（明成化学工業株式会社製））１部との混合水分散体を、実施例１と同様に基材に加工することにより、撥水性布帛を作製した。
[Example 11]
The main component is a woven fabric made of nylon 6 false twisted yarn, and the main component is hydrophilic particles (Snowtex ST-OYL (manufactured by Nissan Chemical Works)) with an average primary particle diameter of 60 nm, which is mainly composed of a silicon compound. A part of a mixed aqueous dispersion (SU-268 (manufactured by Meisei Chemical Works, Ltd.)) of the binder resin to be used is immersed in a base material and then dried, and then a water repellent containing a fluorine-based copolymer as a main component. (AsahiGuard E-SERIES AG-E082 (manufactured by Meisei Chemical Works, Ltd.)) 5 parts and 1 part of a binder resin (polymer FM-1 (manufactured by Meisei Chemical Works, Ltd.)) containing blocked isocyanate as a main component. A water-repellent cloth was prepared by processing the dispersion into a base material in the same manner as in Example 1.
［実施例１２］
ナイロン６仮撚加工糸からなる織物を基材とし、ケイ素化合物とアルミニウム化合物の複合物を主成分とする平均一次粒子径１１０ｎｍの親水性粒子（スノーテックスＳＴ−ＡＫ−ＹＬ（日産化学株式会社製））０．５部、及びブロックドイソシアネートを主成分とするバインダー樹脂（メイカネートＦＭ―１（明成化学工業株式会社製））１部の混合水分散体を、基材に浸漬した後に乾燥させ、次いで、フッ素系共重合物を主成分とする撥水剤（ＡｓａｈｉＧｕａｒｄ Ｅ−ＳＥＲＩＥＳ ＡＧ−Ｅ０８２（明成化学工業株式会社製））５部とブロックドイソシアネートを主成分とするバインダー樹脂（メイカネートＦＭ―１（明成化学工業株式会社製））１部との混合水分散体を、実施例１と同様に基材に加工することにより、撥水性布帛を作製した。
[Example 12]
Hydrophilic particles with an average primary particle diameter of 110 nm (Snowtex ST-AK-YL (manufactured by Nissan Chemical Co., Ltd.)) whose base material is a woven fabric made of nylon 6 false twisted yarn and whose main component is a composite of a silicon compound and an aluminum compound. )) A mixed aqueous dispersion of 0.5 parts and 1 part of a binder resin (Meisei Chemical Works, Ltd.) containing blocked isocyanate as a main component was immersed in a base material and then dried. Next, 5 parts of a water repellent (AsahiGuard E-SERIES AG-E082 (manufactured by Meisei Chemical Works, Ltd.)) containing a fluorine-based copolymer as a main component and a binder resin (Meikanate FM-1) containing blocked isocyanate as a main component. (Manufactured by Meisei Chemical Works, Ltd.)) A water-repellent cloth was produced by processing a mixed aqueous dispersion with one part into a base material in the same manner as in Example 1.
［実施例１３］
ナイロン６生糸からなる織物を基材とし、フッ素系共重合物を主成分とする撥水剤（ＡｓａｈｉＧｕａｒｄ Ｅ−ＳＥＲＩＥＳ ＡＧ−Ｅ０８２（明成化学工業株式会社製））５部、ケイ素化学物とアルミニウム化合物の複合物を主成分とする平均一次粒子径１１０ｎｍの親水性粒子（スノーテックスＳＴ−ＡＫ−ＹＬ（日産化学株式会社製））０．５部、並びにブロックドイソシアネートを主成分とするバインダー樹脂（メイカネートＦＭ―１（明成化学工業株式会社製））１部の混合水分散体を、実施例１と同様に基材に加工することにより、撥水性布帛を作製した。
[Example 13]
5 parts of water repellent (AsahiGuard E-SERIES AG-E082 (manufactured by Meisei Chemical Works, Ltd.)) whose base material is a woven fabric made of 6 nylon yarns and whose main component is a fluorine-based copolymer, silicon chemicals and aluminum compounds. 0.5 parts of hydrophilic particles (Snowtex ST-AK-YL (manufactured by Nissan Chemical Works, Ltd.)) having an average primary particle diameter of 110 nm and a binder resin containing blocked isocyanate as the main component. A water-repellent cloth was prepared by processing one part of a mixed aqueous dispersion of Maycanate FM-1 (manufactured by Meisei Chemical Works, Ltd.) into a base material in the same manner as in Example 1.
［実施例１４］
ナイロン６，６加工糸からなる織物を基材とし、フッ素系共重合物を主成分とする撥水剤（ＡｓａｈｉＧｕａｒｄ Ｅ−ＳＥＲＩＥＳ ＡＧ−Ｅ０８２（明成化学工業株式会社製））５部、ケイ素化合物とアルミニウム化合物の複合物を主成分とする平均一次粒子径１１０ｎｍの親水性粒子（スノーテックスＳＴ−ＡＫ−ＹＬ（日産化学株式会社製））０．５部、並びにブロックドイソシアネートを主成分とするバインダー樹脂（メイカネートＦＭ―１（明成化学工業株式会社製））１部の混合水分散体を、実施例１と同様に基材に加工することにより、撥水性布帛を作製した。
[Example 14]
5 parts of water repellent (AsahiGuard E-SERIES AG-E082 (manufactured by Meisei Chemical Works, Ltd.)) whose base material is a woven fabric made of nylon 6 and 6 processed yarns and whose main component is a fluorine-based copolymer, and a silicon compound. 0.5 parts of hydrophilic particles (Snowtex ST-AK-YL (manufactured by Nissan Chemical Co., Ltd.)) having an average primary particle diameter of 110 nm mainly composed of a composite of an aluminum compound, and a binder containing blocked isocyanate as a main component. A water-repellent cloth was prepared by processing a mixed aqueous dispersion of one part of a resin (Meikanate FM-1 (manufactured by Meisei Chemical Works, Ltd.)) into a base material in the same manner as in Example 1.
［実施例１５］
ポリエステル製不織布を基材とし、フッ素系共重合物を主成分とする撥水剤（ＡｓａｈｉＧｕａｒｄ Ｅ−ＳＥＲＩＥＳ ＡＧ−Ｅ０８２（明成化学工業株式会社製））５部、ケイ素化合物とアルミニウム化合物の複合物を主成分とする平均一次粒子径１１０ｎｍの親水性粒子（スノーテックスＳＴ−ＡＫ−ＹＬ（日産化学株式会社製））０．５部、並びにブロックドイソシアネートを主成分とするバインダー樹脂（メイカネートＦＭ―１（明成化学工業株式会社製））１部の混合水分散体を、実施例１と同様に基材に加工することにより、撥水性布帛を作製した。
[Example 15]
5 parts of a water repellent (AsahiGuard E-SERIES AG-E082 (manufactured by Meisei Chemical Works, Ltd.)) using a polyester non-woven fabric as a base material and a fluorine-based copolymer as a main component, and a composite of a silicon compound and an aluminum compound. 0.5 parts of hydrophilic particles (Snowtex ST-AK-YL (manufactured by Nissan Chemical Works, Ltd.)) with an average primary particle diameter of 110 nm as the main component, and a binder resin (Meisei FM-1) containing blocked isocyanate as the main component. (Manufactured by Meisei Chemical Works, Ltd.)) A water-repellent cloth was prepared by processing a part of the mixed aqueous dispersion into a base material in the same manner as in Example 1.
［比較例１］
ナイロン６仮撚加工糸からなる織物を基材とし、フッ素系共重合物を主成分とする撥水剤（ＡｓａｈｉＧｕａｒｄ Ｅ−ＳＥＲＩＥＳ ＡＧ−Ｅ０８２（明成化学工業株式会社製））５部、ケイ素化合物とアルミニウム化合物の複合物を主成分とする平均一次粒子径１０ｎｍの親水性粒子（スノーテックスＳＴ−ＡＫ（日産化学株式会社製））０．５部、並びにブロックドイソシアネートを主成分とするバインダー樹脂（メイカネートＦＭ―１（明成化学工業株式会社製））１部の混合水分散体を、実施例１と同様に基材に加工することにより、撥水性布帛を作製した。
[Comparative Example 1]
5 parts of water repellent (AsahiGuard E-SERIES AG-E082 (manufactured by Meisei Chemical Works, Ltd.)) whose base material is a woven fabric made of nylon 6 false twisted yarn and whose main component is a fluorine-based copolymer, and a silicon compound. 0.5 parts of hydrophilic particles (Snowtex ST-AK (manufactured by Nissan Chemical Works, Ltd.)) having an average primary particle diameter of 10 nm mainly composed of a composite of an aluminum compound, and a binder resin containing blocked isocyanate as a main component ( A water-repellent cloth was prepared by processing one part of a mixed aqueous dispersion of Maycanate FM-1 (manufactured by Meisei Chemical Works, Ltd.) into a base material in the same manner as in Example 1.
［比較例２］
ナイロン６仮撚加工糸からなる織物を基材とし、フッ素系共重合物を主成分とする撥水剤（ＡｓａｈｉＧｕａｒｄ Ｅ−ＳＥＲＩＥＳ ＡＧ−Ｅ０８２（明成化学工業株式会社製））５部、及びブロックドイソシアネートを主成分とするバインダー樹脂（メイカネートＦＭ―１（明成化学工業株式会社製））１部の混合水分散体を、実施例１と同様に基材に加工することにより、撥水性布帛を作製した。
[Comparative Example 2]
5 parts of water repellent (AsahiGuard E-SERIES AG-E082 (manufactured by Meisei Chemical Works, Ltd.)) whose base material is a woven fabric made of nylon 6 false twisted yarn and whose main component is a fluorine-based copolymer, and blocked. A water-repellent fabric is prepared by processing a mixed aqueous dispersion of one part of a binder resin (Meisei Chemical Works, Ltd.) containing isocyanate as a main component into a base material in the same manner as in Example 1. did.
［比較例３］
ナイロン６仮撚加工糸からなる織物を基材とし、長鎖アルキル重合物を主成分とする撥水剤（メイシールドＺ−１（明成化学工業株式会社製））５部、及びブロックドイソシアネートを主成分とするバインダー樹脂（メイカネートＦＭ―１（明成化学工業株式会社製））１部の混合水分散体を、実施例１と同様に基材に加工することにより、撥水性布帛を作製した。
[Comparative Example 3]
5 parts of a water repellent (Mayshield Z-1 (manufactured by Meisei Chemical Works, Ltd.)) whose base material is a woven fabric made of nylon 6 false twisted yarn and whose main component is a long-chain alkyl polymer, and blocked isocyanate. A water-repellent fabric was prepared by processing a mixed aqueous dispersion of one part of a binder resin (Meisei Chemical Works, Ltd.) as a main component into a base material in the same manner as in Example 1.
［比較例４］
ナイロン６仮撚加工糸からなる織物を基材とし、長鎖アルキル共重合物を主成分とする撥水剤（ネオシードＮＲ−７２００（日華化学株式会社製））５部、及びＮ−メチノールメラミンを主成分とするバインダー樹脂（ＵＮＩＫＡＲＥＳＩＮ ３８０−Ｋ（日華化学株式会社製））１部の混合水分散体を、実施例１と同様に基材に加工することにより、撥水性布帛を作製した。
[Comparative Example 4]
Five parts of a water repellent (Neoseed NR-7200 (manufactured by Nicca Chemical Co., Ltd.)) whose base material is a woven fabric made of nylon 6 false twisted yarn and whose main component is a long-chain alkyl copolymer, and N-methinol. A water-repellent fabric is prepared by processing a mixed aqueous dispersion of a part of a binder resin (UNIKARESIN 380-K (manufactured by Nicca Chemical Co., Ltd.)) containing melamine as a main component into a base material in the same manner as in Example 1. did.
［比較例５］
ナイロン６仮撚加工糸からなる織物を基材とし、シリコーン系共重合物を主成分とする撥水剤（ネオシードＮＲ−８０００（日華化学株式会社製））５部、及びブロックドイソシアネートを主成分とするバインダー樹脂（ＮＫアシストＦＵ（日華化学株式会社製））１部の混合水分散体を、実施例１と同様に基材に加工することにより、撥水性布帛を作製した。
[Comparative Example 5]
Mainly 5 parts of water repellent (Neoseed NR-8000 (manufactured by Nicca Chemical Co., Ltd.)) whose base material is a woven fabric made of nylon 6 false twisted yarn and whose main component is a silicone copolymer, and blocked isocyanate. A water-repellent fabric was produced by processing a mixed aqueous dispersion of one part of a binder resin (NK Assist FU (manufactured by Nicca Chemical Co., Ltd.)) as a component into a base material in the same manner as in Example 1.
［比較例６］
ナイロン６仮撚加工糸からなる織物を基材とし、シリコーン系共重合物を主成分とする撥水剤（ネオシードＮＲ−８０００（日華化学株式会社製））２．５部、及び長鎖アルキル共重合物を主成分とする撥水剤（ネオシードＮＲ−７２００（日華化学株式会社製））２．５部を混合した撥水剤、並びにブロックドイソシアネートを主成分とするバインダー樹脂（ＮＫアシストＦＵ（日華化学株式会社製））１部の混合水分散体を、実施例１と同様に基材に加工することにより、撥水性布帛を作製した。
[Comparative Example 6]
2.5 parts of water repellent (Neoseed NR-8000 (manufactured by Nicca Chemical Co., Ltd.)) whose base material is a woven fabric made of nylon 6 false twisted yarn and whose main component is a silicone-based copolymer, and long-chain alkyl A water repellent containing 2.5 parts of a water repellent containing a copolymer as a main component (Neoseed NR-7200 (manufactured by Nicca Chemical Co., Ltd.)) and a binder resin containing blocked isocyanate as a main component (NK Assist). A water-repellent cloth was prepared by processing a part of the mixed aqueous dispersion of FU (manufactured by Nicca Chemical Co., Ltd.) into a base material in the same manner as in Example 1.
［比較例７］
ナイロン６生糸からなる織物を基材とし、フッ素系共重合物を主成分とする撥水剤（ＡｓａｈｉＧｕａｒｄ Ｅ−ＳＥＲＩＥＳ ＡＧ−Ｅ０８２（明成化学工業株式会社製））５部、及びブロックドイソシアネートを主成分とするバインダー樹脂（メイカネートＦＭ―１（明成化学工業株式会社製））１部の混合水分散体を、実施例１と同様に基材に加工することにより、撥水性布帛を作製した。
[Comparative Example 7]
Mainly 5 parts of water repellent (AsahiGuard E-SERIES AG-E082 (manufactured by Meisei Chemical Works, Ltd.)) whose base material is a woven fabric made of nylon 6 raw yarn and whose main component is a fluorine-based copolymer, and blocked isocyanate. A water-repellent fabric was prepared by processing a mixed aqueous dispersion of one part of a binder resin (Meisei Chemical Works, Ltd.) as a component into a base material in the same manner as in Example 1.
［比較例８］
ナイロン６，６加工糸からなる織物を基材とし、フッ素系共重合物を主成分とする撥水剤（ＡｓａｈｉＧｕａｒｄ Ｅ−ＳＥＲＩＥＳ ＡＧ−Ｅ０８２（明成化学工業株式会社製））５部、及びブロックドイソシアネートを主成分とするバインダー樹脂（メイカネートＦＭ―１（明成化学工業株式会社製））１部の混合水分散体を、実施例１と同様に基材に加工することにより、撥水性布帛を作製した。
[Comparative Example 8]
5 parts of water repellent (AsahiGuard E-SERIES AG-E082 (manufactured by Meisei Chemical Works, Ltd.)) whose base material is a woven fabric made of nylon 6 and 6 processed yarns and whose main component is a fluorine-based copolymer, and blocked. A water-repellent fabric is prepared by processing a mixed aqueous dispersion of one part of a binder resin (Meisei Chemical Works, Ltd.) containing isocyanate as a main component into a base material in the same manner as in Example 1. did.
［比較例９］
ポリエステル製不織布を基材とし、フッ素系共重合物を主成分とする撥水剤（ＡｓａｈｉＧｕａｒｄ Ｅ−ＳＥＲＩＥＳ ＡＧ−Ｅ０８２（明成化学工業株式会社製））５部、及びブロックドイソシアネートを主成分とするバインダー樹脂の混合水分散体（メイカネートＦＭ―１（明成化学工業株式会社製））１部を、実施例１と同様に基材に加工することにより、撥水性布帛を作製した。
[Comparative Example 9]
The main component is a polyester non-woven fabric, 5 parts of a water repellent (AsahiGuard E-SERIES AG-E082 (manufactured by Meisei Chemical Works, Ltd.)) containing a fluorine-based copolymer as a main component, and blocked isocyanate as a main component. A water-repellent cloth was prepared by processing one part of a mixed aqueous dispersion of a binder resin (Meikanate FM-1 (manufactured by Meisei Chemical Works, Ltd.)) into a base material in the same manner as in Example 1.
以上の実施例１〜１５、及び比較例１〜９の成分、原料、特性等を以下の表１に示す。
本発明に係る撥水性布帛は、布帛を構成する繊維（糸）の表面に適切な凹凸形状を有する撥水性被膜が形成されているため、高い撥水性と洗濯耐久性を有する布帛となる、また、該布帛の製造プロセスは、有機溶媒の使用量を低減したものとなる。それゆえ、本発明は、防汚・防水の観点から、良好かつ洗濯耐久性を有する撥水性を備えた布帛、例えば、レインコートやダウンジャケットなどのアパレル製品として、またその製造方法として好適に利用可能である。 The water-repellent fabric according to the present invention is a fabric having high water repellency and washing durability because a water-repellent film having an appropriate uneven shape is formed on the surface of the fibers (threads) constituting the fabric. The fabric manufacturing process reduces the amount of organic solvent used. Therefore, from the viewpoint of antifouling and waterproofing, the present invention is suitably used as a water-repellent fabric having good and washing durability, for example, as an apparel product such as a raincoat or a down jacket, and as a manufacturing method thereof. It is possible.
１ 撥水性布帛
２ 撥水性布帛を構成する繊維
３ 被膜
４ 親水性粒子
５ 撥水剤
６ バインダー樹脂
1 Water-
Claims (8)
親水性粒子、バインダー樹脂原料、及び撥水剤を含む水分散体に布帛を浸漬した後に乾燥させる工程；
を少なくとも１回含む、請求項１、及び３〜５のいずれか１項に記載の撥水性布帛の製造方法。 The following steps:
A step of immersing the fabric in an aqueous dispersion containing hydrophilic particles, a binder resin raw material, and a water repellent, and then drying the fabric;
The method for producing a water-repellent fabric according to any one of claims 1 and 3 to 5, which comprises at least once.
親水性粒子、及びバインダー樹脂原料を含む水分散体に布帛を浸漬した後に乾燥させる工程；
得られた布帛を、バインダー樹脂原料、及び撥水剤を含む水分散体に浸漬した後に乾燥させる工程；
を、それぞれ、少なくとも１回含む、請求項２〜６のいずれか１項に記載の撥水性布帛の製造方法。 The following steps:
A step of immersing the fabric in an aqueous dispersion containing hydrophilic particles and a binder resin raw material and then drying the fabric;
A step of immersing the obtained fabric in an aqueous dispersion containing a binder resin raw material and a water repellent and then drying the fabric;
The method for producing a water-repellent fabric according to any one of claims 2 to 6, each comprising at least once.
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| WO2023068308A1 (en) | 2021-10-20 | 2023-04-27 | ダイキン工業株式会社 | Water repellent composition |
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| JP2006193849A (en) * | 2005-01-12 | 2006-07-27 | Toray Ind Inc | Pollen deposition-proof fiber structure |
| JP2007247089A (en) * | 2006-03-15 | 2007-09-27 | Toray Ind Inc | Fiber structure |
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| US20030100234A1 (en) * | 2000-04-04 | 2003-05-29 | Peter Waeber | Remotely aligned surgical drill guide |
| JP2006193849A (en) * | 2005-01-12 | 2006-07-27 | Toray Ind Inc | Pollen deposition-proof fiber structure |
| JP2007247089A (en) * | 2006-03-15 | 2007-09-27 | Toray Ind Inc | Fiber structure |
| JP2008163471A (en) * | 2006-12-27 | 2008-07-17 | Toray Ind Inc | Fiber structure |
| JP2008163476A (en) * | 2006-12-27 | 2008-07-17 | Toray Ind Inc | Fiber structure |
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