Water-repellent fabric
A non-fluorine-based resin film with an isocyanate compound adheres to the fabric, addressing durability and environmental concerns by maintaining high water repellency after multiple washes.
Patent Information
- Application Number
- JP2025500779
- Authority / Receiving Office
- JP · JP
- Patent Type
- Applications
- Current Assignee / Owner
- Priority Date
- 2022-08-22
- Filing Date
- 2023-08-21
- Publication Date
- 2025-08-15
AI Technical Summary
Existing water-repellent fabrics face issues with durability and environmental friendliness, as fluorine-based compounds are toxic and non-fluorine-based compounds lose water repellency after multiple washes.
A water-repellent fabric with a resin film of 60-100 nm thickness, composed mainly of a non-fluorine-based water-repellent compound and an isocyanate-based compound, where the isocyanate reacts with the fiber to firmly adhere the non-fluorine-based compound, enhancing washing durability.
The fabric maintains excellent water repellency (grade 4 or higher) after 100 washes, with improved durability and environmental safety due to the use of non-toxic compounds.
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Abstract
Description
[Technical Field]
[0001] The present invention relates to a water-repellent fabric that has been treated to be water-repellent. [Background technology]
[0002] As more and more people are going outdoors in pursuit of health, fashion and natural living, outdoor sports clothing fabrics are expected to have excellent water repellency. Currently, water repellents used in water repellent finishing are classified into two types: fluorine-based and non-fluorine-based. Fabrics treated with fluorine-based water repellents have advantages such as high water repellency and high washability. However, the perfluorooctanoic acid ammonium compound (hereinafter referred to as PFOA) and perfluorooctane sulfonate compound (hereinafter referred to as PFOS) contained in fluorine-based water repellents are genotoxic and reproductively toxic, and are difficult to biodegrade, making them unfriendly to environmental protection. For example, Patent Document 1 discloses an easy-to-maintain water and oil repellent, a method for producing the same, and fabrics. Specifically, the fabrics are treated with a water and oil repellent containing polyurethane. Here, polyurethane is obtained by reacting polyisocyanate, fluorosilicone polyol, silicon-containing polyol, other polyols, and blocking agents. Fabrics treated with this water and oil repellent have better water and oil repellency and washability, but the water and oil repellent contains fluorine-based compounds, which do not meet environmental protection requirements. Fabrics treated with environmentally friendly non-fluorinated water repellents have excellent initial water repellency and durability after 10 washes (or 30 washes), but the water repellency significantly decreases after 100 washes. For example, Patent Document 2 discloses a water-repellent-treated fabric and a method for producing the same. Specifically, the surface of the fabric's single fiber is coated with a resin film, and the resin film is primarily composed of a non-fluorinated compound. However, when the fabric is measured using the JIS L1092 spray method, the water repellency is grade 3 or higher after 10 washes, leaving the problem of water repellency decreasing with further washing. Patent Document 3 also discloses a water repellent composition for textiles and a water-repellent textile product. The water repellent composition contains component (A), a silicone resin (B), and water, and component (A) is at least one of a urethane compound (A1), an acrylic acid-based resin (A2), and a reactive silicone (A3). The textile products treated with this water repellent agent only had a water repellency of grade 3 after five washes, and the problem of a decrease in water repellency with increasing number of washes remains unresolved. [Prior art documents] [Patent documents]
[0003] [Patent Document 1] China patent CN106758252A [Patent Document 2] China patent CN105734970A Summary of the Invention [Problem to be solved by the invention]
[0004] An object of the present invention is to provide a fabric that is environmentally friendly and has better water repellency and washing durability. [Means for solving the problem]
[0005] To achieve the above objectives, the technical solutions of the present invention are as follows: The water-repellent fabric of the present invention has a resin film covering the surface of the single fiber constituting the fabric, the resin film having a thickness of 60-100 nm and consisting mainly of a non-fluorine-based water-repellent compound and an isocyanate-based compound. [Effects of the Invention]
[0006] The water-repellent fabric of the present invention has a resin film of a specific thickness coated on the surface of a single fiber, the main components of which are a non-fluorine-based water-repellent compound and an isocyanate-based compound. This resin film makes it difficult for water molecules to penetrate, resulting in excellent initial water repellency. Meanwhile, the isocyanate-based compound in the resin film reacts with the non-fluorine-based water-repellent compound and the fiber, firmly adhering the non-fluorine-based water-repellent compound to the single fiber, thereby improving the washing durability of the fabric. Furthermore, non-fluorine-based compounds are characterized by their high safety and environmental friendliness compared to fluorine-based compounds. DETAILED DESCRIPTION OF THE INVENTION
[0007] The water-repellent fabric of the present invention is coated with a resin film on the surface of the single fiber that constitutes the water-repellent fabric, and the resin film has a thickness of 60-100 nm. If the resin film is less than 60 nm thick, the resin film will be severely damaged after multiple washings, especially after 100 washings, and high washing durability will not be achieved. On the other hand, if the resin film is more than 100 nm thick, the active ingredients will be saturated, and further water repellency improvement will not be achieved, and instead the texture will be affected and costs will increase. It is preferable that the resin film thickness be 70-90 nm, as this range is thought to provide the fabric with excellent washing durability and a good texture.
[0008] In the present invention, the main components of the resin film are a non-fluorine-based water-repellent compound and an isocyanate-based compound. Of these, the non-fluorine-based water-repellent compound forms a film on the surface of the single fiber, imparting good water repellency to the fabric, and the isocyanate group in the isocyanate-based compound reacts not only with the non-fluorine-based water-repellent compound but also with the fiber, thereby firmly adhering the non-fluorine-based water-repellent compound to the single fiber and significantly improving washing durability.
[0009] The isocyanate compound in the resin film of the present invention is preferably a copolymer of aromatic polyfunctional isocyanate and polyol, which has a network structure and can more firmly adhere the non-fluorine-based water-repellent compound, making it less likely to fall off and further improving washing durability.
[0010] The polyol here is not particularly limited and may be a diol and / or triol, and the polyol preferably has a structure represented by formula 1.
[0011] [ka]
[0012] Here, M is an H atom, an alkyl group, an alkoxy group, a hydroxyl group, a hydroxyalkyl group, or a carbonyl group, and 2≦n≦16.
[0013] The terminal groups -OH and -M of the polyol having the structure of Formula 1 are likely to react with the aromatic polyfunctional isocyanate, forming chemical bonds and forming a tight network structure, which is thought to more firmly attach the non-fluorinated water-repellent compound to the fiber and further improve washing durability.
[0014] Preferably, the non-fluorine-based water-repellent compound is a hydrocarbon-based compound, a polysiloxane-based compound A, or a copolymer thereof.
[0015] The hydrocarbon-based compound is not particularly limited and may be an acrylate-based compound, a stearate-based compound, an N-methylol-based compound, etc. Examples of acrylate-based compounds include butyl acrylate, acrylonitrile, acrylamide, etc. Examples of stearate-based compounds include sodium stearate, calcium stearate, aluminum stearate, etc. Examples of N-methylol compounds include etherified hexamethylol melamine, N-hydroxymethyloctadecylamine, etc. Hydrocarbon-based compounds can strengthen the interaction between emulsion particles and water molecules, are advantageous for forming a tightly crosslinked structure, and can improve the strength of the film formed by polymerization on the surface of single fibers.
[0016] When the hydrocarbon compound is an acrylate-based compound, the water-repellent film formed by such a compound has better uniformity, is less susceptible to penetration of water molecules, has a certain rigidity, can withstand the impact of external forces (such as washing or friction), and is less likely to fall off. Preferably, the hydrocarbon compound is an acrylate-based compound, and has a structure represented by Formula 2:
[0017] [ka]
[0018] Here, R1 and R2 are each an alkyl group or an unsaturated hydrocarbon group, and 2≦n≦200.
[0019] The polysiloxane compound A has a low molecular weight and easily penetrates into the interior of the fiber, and the film formed on the surface reduces the coefficient of friction between threads and improves the texture. The polysiloxane compound A having the structure shown in Formula 3 is preferred:
[0020] [ka]
[0021] Here, R3, R4, and R5 are each an alkyl group or an unsaturated hydrocarbon group.
[0022] Preferably, the resin film of the present invention contains a flexible compound, and the flexible compound is a polyethylene-based compound and / or a polysiloxane-based compound B. Due to such compounds, the film formed on the fiber surface has low surface tension and smoothness, which reduces the coefficient of friction between fibers and improves the texture.
[0023] The polysiloxane compound B is not particularly limited, but preferably has a structure represented by formula 4:
[0024] [ka]
[0025] Here, R6 and R7 are each a H atom, an alkyl group or an unsaturated hydrocarbon group, and 2≦n≦200.
[0026] Preferably, the thickness of the resin film on the water-repellent fabric is 40-100 nm after washing 100 times according to the 103 method in the JIS L 0217:1995 standard or the C4M method in the JIS L 1930:2014 standard.
[0027] Preferably, the initial water repellency of the water repellent fabric is grade 4 or higher as measured by the spray method according to JIS L 1092:2009 standard.
[0028] Preferably, the water repellency of the water repellent fabric is grade 3 or higher when measured by the spray method in JIS L 1092:2009 standard after 100 washes according to the 103 method in JIS L 0217:1995 standard or the C4M method in JIS L 1930:2014 standard.
[0029] The water-repellent fabric of the present invention may be made of any fiber material, including cellulose and / or synthetic fibers. The cellulose fibers used herein include natural cellulose fibers and regenerated cellulose fibers. Examples of natural fibers include cotton and hemp. Examples of regenerated cellulose fibers include viscose and mullite. Examples of synthetic fibers include polyester (PET), polyamide, and polyacrylonitrile.
[0030] The water-repellent fabric of the present invention may be a woven fabric or a knitted fabric. The weave of the woven fabric is not particularly limited, but may be plain weave, twill weave, satin weave, etc. The weave of the knitted fabric is also not particularly limited, but may be weft flat needle, rib, front and back, warp flat needle, satin, etc.
[0031] The method for producing the water-repellent fabric of the present invention is not particularly limited, but the product of the present invention can be obtained by a method in which the fabric is subjected to pretreatment (de-sizing and scouring), intermediate shaping, dyeing (optional), and finishing.
[0032] Here, the finishing process is preferably performed by immersing the material in a processing solution having the following composition, squeezing it, drying it at a temperature of 80 to 150°C, and finally curing it at a temperature of 130 to 200°C.
[0033] The processing solution for the immersion treatment has the following composition: Water repellent 10~200g / L Crosslinking agent 5~50g / L Fabric softener 0~40g / L Penetrant 5-30g / L The rest is water.
[0034] Here, the fabric weight is 50-300g / m 2 If the basis weight is less than 50 g / m², the requirements for the weaving process become too high, and there is a risk of phenomena such as thread breakage occurring, which is disadvantageous for production and is therefore undesirable. 2 If the thickness exceeds this range, it is not preferable because it may affect the wearing comfort.
[0035] The water repellent agent used here is a non-fluorine-based water repellent agent, and although the type is not particularly limited, it is preferably one or more of hydrocarbon compounds, paraffin compounds, and polysiloxane compounds A. The amount used is preferably 40 to 100 g / L. If the amount used is less than 40 g / L, it is difficult to form a uniform water-repellent film on the fiber surface, resulting in poor water repellency, which is undesirable. If the amount used exceeds 100 g / L, the active ingredient coated on the fiber surface will already be saturated, making it impossible to further improve water repellency, and will instead affect the texture and increase costs, which is undesirable.
[0036] The type of crosslinking agent used here is not particularly limited, but a blocked isocyanate is preferred, and a polymer composed of an aromatic polyfunctional isocyanate and a polyol is more preferred. The amount used is preferably 10 to 40 g / L. Amounts less than 10 g / L result in fewer reactive groups that react with the water repellent and adhere to the fiber surface, and after multiple washes, especially 100 washes, the isocyanate attached to the water repellent falls off, resulting in the fabric not having ultra-high washing durability, which is undesirable. Amounts greater than 40 g / L are undesirable because the active ingredient that reacts with the water repellent reaches saturation, preventing further improvement in washing durability and adversely affecting texture and increasing costs.
[0037] The type of softener used here is not particularly limited, but is preferably a polyethylene-based compound and / or a polysiloxane-based compound B. The amount used is preferably 10 to 30 g / L. If the amount used is less than 10 g / L, it is difficult to form a uniform soft film on the fiber surface, making it difficult to improve the texture, which is not preferred, while if the amount used exceeds 30 g / L, the effect of improving the texture is not noticeable and the water repellency of the fabric may decrease, which is also not preferred.
[0038] The type of penetrating agent used here is not particularly limited, but isopropyl alcohol and / or aliphatic ethoxylated alcohol is preferred. The amount used is preferably 10 to 20 g / L. If the amount used is less than 10 g / L, the agent will not penetrate easily between the fibers, making it difficult to form a uniform water-repellent film between the fibers, and water molecules may penetrate and affect the water repellency, which is not preferred. If the amount used is more than 20 g / L, the active ingredient will be saturated, which is not preferred, as it increases costs.
[0039] The above agents may be commercially available or may be synthesized according to techniques known in the art.
[0040] At drying temperatures of 80°C or higher, the water-repellent agent forms a film, achieving water-repellent properties. At curing temperatures of 130°C or higher, a chemical reaction with the crosslinking agent occurs, firmly adhering the film to the fabric, giving the fabric both water-repellent properties and washing durability.
[0041] The method for preparing the processing solution is not particularly limited, and involves sequentially adding a water repellent and a crosslinking agent, then adding a softener if necessary to improve the texture, and mixing with water while continuously stirring at a moderate speed so as not to inhibit the emulsification effect. During actual processing, the fabric, processing agents, and amounts used must be adjusted according to the type of fiber being processed, and local adjustments to the processing method can be made in a timely manner to maximize the functionality of the processing solution and improve the performance of the fabric. [Example]
[0042] The present invention will be described in detail below with reference to examples and comparative examples.
[0043] Each parameter according to the present invention is measured by the following method.
[0044] (1) Confirmation of the water repellency of the fabric and the fluorine content in the resin film 1) A 5cm x 2cm sample was taken and fixed in a holder according to DB44 / T 1872-2016, a standard for testing the wettability of fabric surfaces (contact angle method). The holder with the sample attached was then placed on the test bench of the contact angle measuring instrument, and the needle was adjusted to a height of 10mm from the surface of the sample fabric. A 5μL droplet was placed on the sample surface, and after 60 seconds of contact, the sample and the droplet on its surface were photographed. If the contact angle θ was greater than 0°, the sample was determined to be a fabric containing a water-repellent compound.
[0045] 2) Then, take a sample measuring 1cm x 1cm, scan the surface of the sample using an elemental analyzer, and measure the fluorine content. If the measured fluorine content is 0, it is determined that the resin film contains non-fluorine compounds.
[0046] (2) Resin film thickness A. Sampling and Measurement Take a sample measuring 1 cm x 1 cm, cut it along a position perpendicular to the warp or weft direction of the fabric to obtain a cross section, and observe the cross section using the equipment below to measure the thickness of the resin film deposited on the fabric surface. If necessary, select one of the equipment below to perform the measurement. Equipment 1: Model number: Hitachi REGULUS-8100 scanning electron microscope Measurement conditions: No gold plating, 1kV voltage deceleration mode For operating procedures, refer to JY T010-1996 "General Rules for Analytical Scanning Electron Microscopy." Equipment 2: Model number: JEOL JEM-2200FS 200kV energy filter field emission electron microscope Measurement conditions: RuO4 stained ultrathin sections, accelerating voltage: 200 kV The operating method is based on KS / D 8544-2006 "Metal Coating Layer / Paint Film Thickness Measurement / Transmission Electron Microscopy" B. Calculation 1) Calculate the single fiber diameter d using the following formula:
[0047] [ka]
[0048] d: Single fiber diameter (cm) γ: Fiber density (g / cm 3 ) Ndt: Fiber fineness (dtex) 2) Point A is taken at any position on the surface of the cross section of a single fiber. 3) Create a circle with point A as its center and a radius 0.1 times the diameter d of the single fiber, and the circle intersects with the surface of the single fiber cross section at point B. 4) Using points A and B as contact points, tangent lines drawn on the surface of the cross section of the single fiber intersect at point O, and the interior angle θ of the intersection is measured. 5) If 90°≦θ<178°, use O as the end point and draw a bisector of θ° / 2 at the interior angle ∠AOB. The bisector intersects the surface of the single fiber cross section at point E, and measure the film thickness at point E. 6) Repeat steps 1) to 5) above to measure a total of five times, i.e., measure five times at different positions on the same sample, and take the average of the five sets of data to determine the thickness of the resin film of the present invention.
[0049] (3) Qualitative analysis of compounds in resin films 1) Sampling and measurement Two 10cm x 10cm samples were taken. Qualitative analysis was performed using a Fourier transform attenuated total reflection infrared spectrometer. The operating method was based on GB / T 6040-2002 "General Rules for Infrared Spectroscopic Analysis Methods." The measurement parameters were: ATR crystal: Ge, incident angle: 45°, measurement range: 4000-680cm -1 A sample cloth is placed directly on the reflective surface of the Ge crystal of the Fourier transform attenuated total reflection infrared spectrometer, and the wavelength is 4000 to 680 cm -1 The surface of the remaining sample is wiped with a cotton ball containing carbon tetrachloride reagent, and then the sample is applied to a potassium bromide wafer crystal and measured to obtain spectrum Y.
[0050] 2) Analyze the data.
[0051] Based on Spectrum X, 1725 cm -1 , 1250cm -1 , 1200~1150cm -1 and 1125-1100cm -1 There is a characteristic absorption peak at 1725 cm -1 and 1200-1150cm -1 If there is a strong absorption peak between 2953.1 cm, it is determined that an acrylic compound is present. -1 , 2921.0cm -1 , 2853.3cm -1 , 1456.9cm -1 , 1376.9cm -1 , 722.7cm -1 There is a characteristic absorption peak around 2953.1 cm -1 and 2921.0 cm -1 If there is a strong absorption peak around 1420cm, it is determined that a paraffinic compound is present. -1 There is a weak absorption band near 1265-1270 cm -1 There is a sharp, strong absorption peak around 1087 cm -1 and 1020cm -1 If there is a strong absorption band near 1563 cm, it is determined that polysiloxane compound B is present. -1 , 816cm -1 If there is a characteristic absorption peak in the vicinity, it is determined that an isocyanate compound is present.
[0052] Spectrum Y, 1458cm -1 There is a weak absorption peak around 827 cm -1 , 1091cm -1 , 1193cm -1 , 2840cm -1 , 2941cm -1 If there is a sharp, strong absorption peak in the vicinity of 1200 to 700 cm, it is determined that polysiloxane compound A is present. -1 There is one weak absorption peak in the region of 2960–2850 cm -1 There is a strong absorption peak at 1275-1020cm -1If there is one absorption peak in the region, it is determined that a polyol is present.
[0053] (4) Qualitative analysis of polyol formula 1 structure 1) Sampling A 10g sample was taken, cut into pieces, and then placed in a reactor. The treatment conditions were a temperature of 250-340°C, a pressure of 50-150KPa, and a catalyst of an alkali metal hydroxide such as sodium hydroxide to obtain a mixture containing polyol. The mixture containing polyol was extracted and separated with an organic solvent, N,N-dimethylformamide, and dried to obtain polyol crystals.
[0054] 2) Measurement The separated and extracted polyol crystals were analyzed by elemental analysis using an EDS spectrometer (model number: OXFORD INSTRUMENTS XPLORE), an infrared spectrum was obtained using a Fourier transform attenuated total reflection infrared spectrometer, and a carbon spectrum ( 13 C NMR) chart and hydrogen spectrum ( 1 1 H NMR charts can be obtained to determine whether a polyol containing the structure of Formula 1 is present.
[0055] (5) Water repellency Measurements are made in accordance with JIS L1092:2009 standards.
[0056] (6) Laundry Wash 100 times in accordance with the 103 method in the JIS L0217:1995 standard or the C 4M method in the JIS L1930:2014 standard.
[0057] (7) Texture The bending resistance of a fabric is measured in accordance with JIS L10962010: Method A (cantilever method). The lower the bending resistance value, the softer the fabric.
[0058] The resins used in the examples and comparative examples are as follows. (1) Water repellent A: A copolymer of hydrocarbon compounds and polysiloxane compounds, the product name is RUCO-DRY DHT, and the manufacturer is Rudolph. (2) Water repellent B: Polysiloxane, product name NEOSEED NR-8800, manufacturer Nicca Chemical (China) Co., Ltd. (3) Water repellent C: Pyridine quaternary ammonium salts, trade name PF, manufactured by Changsha Jianglong Chemical Technology Co., Ltd. (4) Crosslinking agent A: Self-made polymer consisting of aromatic isocyanate compound and polyol The structural formula of the aromatic isocyanate compound is as follows:
[0059] [ka]
[0060] The structural formula of the polyol is as follows:
[0061] [ka]
[0062] (5) Crosslinking agent B: aliphatic isocyanates, trade name FB-12, manufactured by Shanghai Simheng Polymer Materials Co., Ltd. (6) Crosslinking agent C: Aromatic isocyanates (not including polyols), trade name XDI, manufactured by Mitsui Chemicals, Inc. (7) Crosslinking agent D: Melamine-based, product name M-3, manufacturer: DIC Corporation. (8) Crosslinking agent E: Self-produced, a polymer consisting of an aromatic isocyanate compound and a polyol.
[0063] The structural formula of the aromatic isocyanate compound is as follows:
[0064] [ka]
[0065] The structural formula of the polyol is as follows:
[0066] [ka]
[0067] (9) Fabric softener A: Polysiloxane, product name S-1723, manufactured by Nantong Dongrou Industrial Trading Co., Ltd. (10) Fabric softener B: Polyethylene, product name RUCO-LUB KSA, manufacturer Rudolph Chemical Co., Ltd. (11) Penetrating agent: isopropyl alcohol, product name Texas BG-2, manufacturer: Regal Nicca Chemical Co., Ltd.
[0068] Example 1 A plain weave fabric with a density of 200 x 170 threads per inch and made of 100% polyester fiber was selected and subjected to the usual pretreatment (de-sizing and scouring), dyeing (disperse dye at 130°C for 45 minutes), intermediate setting (170°C for 1 minute), and finishing to obtain a water-repellent fabric of the present invention. The test result parameters are shown in Table 1.
[0069] The specific conditions for post-finishing are one dip and one nip, with a pick-up rate of approximately 80%, followed by heat treatment at 130°C for 2 minutes, and finally set at 170°C for 1 minute. The immersion processing solution is composed of the following components: Water repellent A 70g / L Crosslinker A 30g / L Fabric softener A 10g / L Penetrating agent 10g / L The rest is water.
[0070] Example 2 The water-repellent fabric of the present invention was obtained in the same manner as in Example 1, except that the dipping solution consisted of the following components: The test result parameters are shown in Table 1. Water repellent A 100g / L Crosslinker A 30g / L Fabric softener A 10g / L Penetrating agent 10g / L The rest is water.
[0071] Example 3 The water-repellent fabric of the present invention was obtained in the same manner as in Example 1, except that the dipping solution consisted of the following components: The test result parameters are shown in Table 1. Water repellent A 70g / L Crosslinker B 30g / L Fabric softener A 10g / L Penetrating agent 10g / L The rest is water.
[0072] Example 4 The water-repellent fabric of the present invention was obtained in the same manner as in Example 1, except that the dipping solution consisted of the following components: The test result parameters are shown in Table 1. Water repellent A 70g / L Crosslinker A 30g / L Penetrating agent 10g / L The rest is water.
[0073] Example 5 The water-repellent fabric of the present invention was obtained in the same manner as in Example 1, except that the dipping solution consisted of the following components: The test result parameters are shown in Table 1. Water repellent B 70g / L Crosslinker A 30g / L Fabric softener A 10g / L Penetrating agent 10g / L The rest is water.
[0074] Example 6 The water-repellent fabric of the present invention was obtained in the same manner as in Example 1, except that the dipping solution consisted of the following components: The test result parameters are shown in Table 1. Water repellent C 70g / L Crosslinker A 30g / L Fabric softener A 10g / L Penetrating agent 10g / L The rest is water.
[0075] Example 7 The water-repellent fabric of the present invention was obtained in the same manner as in Example 1, except that the dipping solution consisted of the following components: The test result parameters are shown in Table 1. Water repellent B 70g / L Crosslinker A 30g / L Fabric softener B 10g / L Penetrating agent 10g / L The rest is water.
[0076] Example 8 The water-repellent fabric of the present invention was obtained in the same manner as in Example 1, except that the dipping solution consisted of the following components: The test result parameters are shown in Table 1. Water repellent A 150g / L Crosslinker A 30g / L Fabric softener A 10g / L Penetrating agent 10g / L The rest is water.
[0077] Example 9 The water-repellent fabric of the present invention was obtained in the same manner as in Example 1, except that the dipping solution consisted of the following components: The test result parameters are shown in Table 2. Water repellent A 30g / L Crosslinker A 30g / L Fabric softener A 10g / L Penetrating agent 10g / L The rest is water.
[0078] Example 10 The water-repellent fabric of the present invention was obtained in the same manner as in Example 1, except that the dipping solution consisted of the following components: The test result parameters are shown in Table 2. Water repellent A 70g / L Crosslinker A 10g / L Fabric softener A 10g / L Penetrating agent 10g / L The rest is water.
[0079] Example 11 The same procedure as in Example 1 was carried out except that the dipping solution consisted of the following components. The test result parameters for the water-repellent fabric of the present invention are shown in Table 2. Water repellent A 70g / L Crosslinker A 50g / L Fabric softener A 10g / L Penetrating agent 10g / L The rest is water.
[0080] Example 12 The water-repellent fabric of the present invention was obtained in the same manner as in Example 1, except that the dipping solution consisted of the following components: The test result parameters are shown in Table 2. Water repellent A 30g / L Crosslinker A 30g / L Fabric softener A 30g / L Penetrating agent 10g / L The rest is water.
[0081] Example 13 The water-repellent fabric of the present invention was obtained in the same manner as in Example 1, except that the dipping solution consisted of the following components. Specific test result parameters are shown in Table 2. Water repellent A 70g / L Crosslinker C 30g / L Fabric softener A 10g / L Penetrating agent 10g / L The rest is water.
[0082] Example 14 The water-repellent fabric of the present invention was obtained in the same manner as in Example 1, except that the dipping solution consisted of the following components: The test result parameters are shown in Table 2. Water repellent A 70g / L Crosslinker E 30g / L Fabric softener A 10g / L Penetrating agent 10g / L The rest is water.
[0083] Comparative Example 1 A water-repellent fabric was obtained in the same manner as in Example 1, except that the dipping solution consisted of the following components: The test result parameters are shown in Table 2. Water repellent A 70g / L Crosslinker A 10g / L Penetrating agent 10g / L The rest is water.
[0084] Comparative Example 2 A water-repellent fabric was obtained in the same manner as in Example 1, except that the dipping solution consisted of the following components: The test result parameters are shown in Table 2. Water repellent A 70g / L Crosslinker D 30g / L Fabric softener A 10g / L Penetrating agent 10g / L The rest is water.
[0085] [Table 1]
[0086] [Table 2]
[0087] According to Tables 1 and 2, (1) From the results of Examples 1 and 3, it was found that the water-repellent fabrics obtained by processing using a crosslinking agent obtained by reacting a polyol with an aromatic isocyanate under the same conditions had the same initial water-repellent properties and texture as the water-repellent fabrics obtained by processing using an aliphatic isocyanate crosslinking agent, but the water-repellent properties of the former after 100 washes were superior to those of the latter. (2) From Examples 1 and 4, it was found that under the same conditions, the water-repellent fabric obtained by fabric softener treatment had the same level of water repellency before and after washing as the water-repellent fabric obtained without fabric softener treatment, but the texture of the former was superior to that of the latter. (3) From the results of Examples 1 and 5, it was found that the water-repellent fabrics obtained by treating with a copolymer of a hydrocarbon compound and a polysiloxane compound under the same conditions had the same initial water repellency as the water-repellent fabrics obtained by treating with a polysiloxane water repellent, and although the texture of the former was slightly inferior to that of the latter, its water repellency after 100 washes was superior to that of the latter. (4) From the results of Examples 1 and 6, it was found that the water-repellent fabrics obtained by treating with a copolymer of a hydrocarbon compound and a polysiloxane compound under the same conditions had the same initial water repellency and texture as the water-repellent fabrics obtained by treating with a pyridine quaternary ammonium salt water repellent, but the water repellency of the former after 100 washes was superior to that of the latter. (5) From Example 1 and Example 14, it was found that the water-repellent fabric obtained by processing using crosslinker A (a polyol containing the structure of Formula 1) under the same conditions was compared with the water-repellent fabric obtained by processing using crosslinker E (a polyol not containing the structure of Formula 1) under the same conditions. The initial water repellency and texture of both fabrics were at the same level, but the water repellency of the former after 100 washes was superior to that of the latter. (6) From Comparative Example 1 and Example 13, it was found that the fabric obtained without using a crosslinking agent under the same conditions had relatively good initial water repellency and texture compared to the fabric obtained using an aromatic isocyanate-based crosslinking agent (not containing polyol), but the water repellency after 100 washes was only grade 2. (7) From Comparative Example 2 and Example 13, it was found that the fabric obtained by processing using a melamine-based crosslinking agent under the same conditions had relatively good initial water repellency compared to the fabric obtained by processing using an aromatic isocyanate-based crosslinking agent (not containing polyol), but the water repellency after 100 washes was only grade 2.
Claims
1. A water-repellent fabric characterized in that the surface of the single fiber constituting the water-repellent fabric is coated with a resin film, the resin film has a thickness of 60 to 100 nm, and the main components of the resin film are a non-fluorine-based water-repellent compound and an isocyanate-based compound.
2. 2. The water-repellent fabric according to claim 1, wherein the isocyanate compound is a polymer composed of an aromatic polyfunctional isocyanate and a polyol.
3. 3. The water-repellent fabric according to claim 2, wherein the polyol is a compound having the structure of Formula 1, where M is an H atom, an alkyl group, an alkoxy group, a hydroxy group, a hydroxyalkyl group, or a carbonyl group, and 2≦n≦16. 【Chemical 1】
4. 2. The water-repellent fabric according to claim 1, wherein the non-fluorine-based water-repellent compound is a hydrocarbon-based compound, a polysiloxane-based compound A, or a copolymer thereof.
5. 5. The water-repellent fabric according to claim 4, wherein the hydrocarbon-based compound is an acrylic compound having the structure of Formula 2, where R1 and R2 are each an alkyl group or an unsaturated hydrocarbon group, and 2≦n≦200. 【Chemistry 2】
6. 5. The water-repellent fabric according to claim 4, wherein the polysiloxane compound A is a compound having a structure of Formula 3, where R3, R4, and R5 are each an alkyl group or an unsaturated hydrocarbon group. 【Chemistry 3】
7. 2. The water-repellent fabric according to claim 1, wherein the resin film contains a flexible compound, and the flexible compound is a polyethylene-based compound and / or a polysiloxane-based compound B.
8. 8. The water-repellent fabric according to any one of claims 1 to 7, characterized in that after being washed 100 times according to the 103 method in the JIS L 0217:1995 standard or the C4M method in the JIS L 1930:2014 standard, the thickness of the resin film on the water-repellent fabric is 40 to 100 nm.
9. 8. The water-repellent fabric according to any one of claims 1 to 7, characterized in that the initial water repellency of the fabric is grade 4 or higher as measured by the spray method according to the JIS L 1092:2009 standard.
10. 8. The water-repellent fabric according to any one of claims 1 to 7, characterized in that the water-repellency of the fabric is grade 3 or higher as measured by the spray method in accordance with the JIS L 1092:2009 standard after 100 washes according to the 103 method in accordance with the JIS L 0217:1995 standard or the C4M method in accordance with the JIS L 1930:2014 standard.
Citation Information
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